DIN EN ISO 4829-2-2016 Steels - Determination of total silicon contents - Reduced molybdosilicate spectrophotometric method - Part 2 Silicon contents between 0 01 % and 0 05 % (ISO.pdf

1、August 2016 English price group 10No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 77.040.30!%Y.P“2541145www.din.deD

2、IN EN ISO 4829-2Steels Determination of total silicon contents Reduced molybdosilicate spectrophotometric method Part 2: Silicon contents between 0,01 % and 0,05 % (ISO 4829-2:2016);English version EN ISO 4829-2:2016,English translation of DIN EN ISO 4829-2:2016-08Stahl Bestimmung des Gesamtsilicium

3、anteils Spektrophotometrisches Verfahren mit reduziertem Molybdatosilicat Teil 2: Siliciumanteile zwischen 0,01 % und 0,05 % (ISO 4829-2:2016);Englische Fassung EN ISO 4829-2:2016,Englische bersetzung von DIN EN ISO 4829-2:2016-08Aciers Dtermination du silicium total Mthode spectrophotomtrique au si

4、licomolybdate rduit Partie 2: Teneurs en silicium comprises entre 0,01 % et 0,05 % (ISO 4829-2:2016);Version anglaise EN ISO 4829-2:2016,Traduction anglaise de DIN EN ISO 4829-2:2016-08SupersedesDIN EN 24829-2:1992-10www.beuth.deDocument comprises 16 pagesDTranslation by DIN-Sprachendienst.In case o

5、f doubt, the German-language original shall be considered authoritative.08.16 DIN EN ISO 4829-2:2016-08 2 A comma is used as the decimal marker. National foreword This document (EN ISO 4829-2:2016) has been prepared by Technical Committee ISO/TC 17 “Steel” in collaboration with Technical Committee E

6、CISS/TC 102 “Methods of chemical analysis for iron and steel” (Secretariat: SIS, Sweden). The responsible German body involved in its preparation was DIN-Normenausschuss Eisen und Stahl (DIN Standards Committee Iron and Steel), Working Committee NA 021-00-30 AA Analysenverfahren. The DIN Standards c

7、orresponding to the International Standards referred to in this document are as follows: ISO 648 DIN EN ISO 648 ISO 1042 DIN EN ISO 1042 ISO 3696 DIN ISO 3696 ISO 5725*)DIN ISO 5725*)ISO 14284 DIN EN ISO 14284 Amendments This standard differs from DIN EN 24829-2:1992-10 as follows: a) the standard h

8、as been issued in collaboration with CEN as an ISO Standard in the parallel voting procedure; b) the standard has been editorially revised. Previous editions DIN EN 24829-2: 1992-10 National Annex NA (informative) Bibliography DIN EN ISO 648, Laboratory glassware Single-volume pipettes DIN EN ISO 10

9、42, Laboratory glassware One-mark volumetric flasks DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 5725, Precision of test methods Determination of repeatability and reproducibility for a standard test method by interlaboratory tests*)DIN EN ISO 14284, Steel

10、 and iron Sampling and preparation of samples for the determination of chemical composition *)Has been replaced by the ISO 5725 standards series. *)Has been replaced by the DIN ISO 5725 standards series. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4829-2 March 2016 ICS 77.080.01 Superse

11、des EN 24829-2:1990English Version Steels - Determination of total silicon contents - Reduced molybdosilicate spectrophotometric method - Part 2: Silicon contents between 0,01 % and 0,05 %(ISO 4829-2:2016) Aciers - Dtermination du silicium total - Mthode spectrophotomtrique au silicomolybdate rduit

12、- Partie 2: Teneurs en silicium comprises entre0,01 % et0,05 % (ISO 4829-2:2016) Stahl - Bestimmung des Gesamtsiliciumanteils - Spektrophotometrische Methode mit reduziertem Molybdatosilicat - Teil 2: Siliciumanteile zwischen0,01% und 0,05 % (ISO 4829-2:2016) This European Standard was approved by C

13、EN on 21 November 2015. 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 without any alteration. Up-to-date lists and bibliographical references concerning such national standa

14、rds may be obtained on application to the CEN-CENELEC 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 translation under the responsibility of a CEN member into its own language and not

15、ified 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, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, I

16、celand, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Man

17、agement Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4829-2:2016 EForeword .41 Scope . 52 Normative references 53 Principle 54 Reagents 55 Apparatus . 76 Sampling 87 Procedure.

18、87.1 Test portion 87.2 Blank test . 87.3 Determination . 87.3.1 Dissolution of the test portion . 87.3.2 Treatment of insoluble residue . 87.3.3 Preparation of the test solution 87.3.4 Development of the colour 97.3.5 Spectrophotometric measurements . 97.4 Establishment of the calibration curve . 10

19、7.4.1 Preparation of the calibration solutions . 107.4.2 Spectrophotometric measurements 107.4.3 Plotting of the calibration curve 108 Expression of results . 108.1 Method of calculation . 108.2 Precision 119 Test report 11Annex A (informative) Additional information on the interlaboratory test 13Bi

20、bliography .14Contents Page2EN ISO 4829-2:2016 (E) DIN EN ISO 4829-2:2016-08 European foreword .3European foreword This document (EN ISO 4829-2:2016) has been prepared by Technical Committee ISO/TC 17 “Steel” in collaboration with Technical Committee ECISS/TC 102 “Methods of chemical analysis for ir

21、on and steel” the secretariat of which is held by SIS. 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 September 2016, and conflicting national standards shall be withdrawn at the latest by Septem

22、ber 2016. 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 document supersedes EN 24829-2:1990. This document has been prepared un

23、der a mandate given to CEN by the European Commission and the European Free Trade Association. 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, Croatia, Cyprus

24、, 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United K

25、ingdom. Endorsement notice The text of ISO 4829-2:2016 has been approved by CEN as EN ISO 4829-2:2016 without any modification. 3EN ISO 4829-2:2016 (E) DIN EN ISO 4829-2:2016-08 ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (I

26、SO 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 on that committee. International organizations, gov

27、ernmental 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.The procedures used to develop this document and those intended for its further mainte

28、nance 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 rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attent

29、ion 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 identified during the development of the document will be in the Introduction

30、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 on the meaning of ISO specific terms and expressions related to conformity

31、 assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information.The committee responsible for this document is ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of chemical

32、 composition.This second edition cancels and replaces the first edition (ISO 4829-2:1988), which has been technically revised.ISO 4829 consists of the following parts, under the general title Steels Determination of total silicon contents Reduced molybdosilicate spectrophotometric method: Part 1: Si

33、licon contents between 0,05 % and 1,0 % Part 2: Silicon contents between 0,01 % and 0,05 %4EN ISO 4829-2:2016 (E) DIN EN ISO 4829-2:2016-08 1 ScopeThis part of ISO 4829 specifies a spectrophotometric method for the determination of total silicon in steels using reduced molybdosilicate.The method is

34、applicable to silicon contents between 0,01 % and 0,05 % (mass fraction) in steels.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For unda

35、ted references, the latest edition of the referenced document (including any amendments) applies.ISO 648, Laboratory glassware Single-volume pipettesISO 1042, Laboratory glassware One-mark volumetric flasksISO 3696, Water for analytical laboratory use Specification and test methodsISO 14284, Steel a

36、nd iron Sampling and preparation of samples for the determination of chemical composition3 PrincipleDissolution of a test portion in a hydrochloric/nitric acids mixture.Fusion of the acid-insoluble residue with sodium peroxide. Formation of the oxidized molybdosilicate (yellow) complex in weak acid

37、solution.Selective reduction of the molybdosilicate complex to a blue complex with ascorbic acid, after increasing the sulphuric acid concentration and adding oxalic acid to prevent the interference of phosphorus, arsenic and vanadium.Spectrophotometric measurement of the reduced blue complex at a w

38、avelength of about 810 nm.4 ReagentsDuring the analysis, 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.Reage

39、nts supplied in glass bottles, once opened, might absorb 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

40、 opened bottles of all reagents be used for the preparation of reagent solutions.5EN ISO 4829-2:2016 (E) DIN EN ISO 4829-2:2016-08 To avoid adventitious contamination, the water shall be prepared, as required, for the specific purpose and collected in polypropylene containers for immediate use.All s

41、olutions shall be freshly prepared and stored in polypropylene or polytetrafluoroethylene containers.4.1 Pure iron, silicon content less than 2 g/g.4.2 Sodium peroxide, particle size less than 500 m.4.3 Sulphuric acid, approximately 1,84 g/ml, diluted 1 + 3.Add cautiously, while stirring, 250 ml of

42、sulphuric acid, approximately 1,84 g/ml to 600 ml of water. Cool, dilute to 1 l with water and mix.4.4 Sulphuric acid, approximately 1,84 g/ml, diluted 1 + 19.Add cautiously, while stirring, 50 ml of sulphuric acid, approximately 1,84 g/ml to 800 ml of water. Cool, dilute to 1 l with water and mix.4

43、.5 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.4.6 Ascorbic acid, 20 g/l solution.This solution shall be freshly prepared.4.7 Oxalic acid, 50 g

44、/l solution.Dissolve 5 g of oxalic acid di-hydrate (C2H2O42H2O) in water, dilute to 100 ml with water and mix.4.8 Hydrogen peroxide, 60 g/l solution.Dilute 200 ml of hydrogen peroxide, 300 g/l, to 1 l with water and mix.4.9 Potassium permanganate, 22,5 g/l solution.This solution shall be filtered be

45、fore use in order to remove the fine particles of MnO2 that may be present in the solution, as they will interfere with the measurement.4.10 Sodium molybdate, 25 g/l solution.Dissolve 2,5 g of sodium molybdate di-hydrate (Na2MoO42H2O) in 50 ml of water and filter through a medium-texture filter pape

46、r.Immediately before use, add 15 ml of sulphuric acid (4.4), dilute to 100 ml with water and mix.4.11 Silicon standard solution, 1 g/l.Prepare a 1 g/l silicon standard solution by using one of the procedures described in 4.11.1 or 4.11.2.4.11.1 Preparation with silicaWeigh to the nearest 0,1 mg, 2,1

47、39 3 g of freshly calcined high-purity silica ( 99,9 % SiO2) and transfer to a platinum crucible.6EN ISO 4829-2:2016 (E) DIN EN ISO 4829-2:2016-08 The high-purity 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 anhydrous sodiu

48、m carbonate 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, into a 1 000 ml one-mark

49、 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.4.11.2 Preparation with ammonium hexafluorosilicateDry several grams of ammonium 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