DIN EN ISO 15350-2010 Steel and iron - Determination of total carbon and sulfur content - Infrared absorption method after combustion in an induction furnace (routine method) (ISO .pdf

1、August 2010 Translation by DIN-Sprachendienst.English price group 14No 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

2、 77.080.01!$j6“1711957www.din.deDDIN EN ISO 15350Steel and iron Determination of total carbon and sulfur content Infrared absorption method after combustion in an induction furnace(routine method) (ISO 15350:2000)English translation of DIN EN ISO 15350:2010-08Stahl und Eisen Bestimmung der Gesamtgeh

3、alte an Kohlenstoff und Schwefel Infrarotabsorptionsverfahren nach Verbrennung in einem Induktionsofen(Standardverfahren) (ISO 15350:2000)Englische bersetzung von DIN EN ISO 15350:2010-08Aciers et fontes Dosage du carbone et du soufre totaux Mthode par absorption dans linfrarouge aprs combustion dan

4、s un four induction(mthode pratique) (ISO 15350:2000)Traduction anglaise de DIN EN ISO 15350:2010-08www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 30 pages07.10 DIN EN ISO 15350:2010-08 2 A comma is used as the decimal marker. National

5、 foreword This standard has been prepared by Technical Committee ISO/TC 17 “Steel” and has been taken over by Technical Committee ECISS/TC 102 “Methods of chemical analysis for iron and steel” (Secretariat: SIS, Sweden) as a European Standard without any modification. The responsible German body inv

6、olved in its preparation was the Normenausschuss Eisen und Stahl (Iron and Steel Standards Committee), Working Committee NA 021-00-30 AA Analyseverfahren. There is no national standard on the subject. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15350 April 2010 ICS 77.080.01 English Ver

7、sion Steel and iron - Determination of total carbon and sulfur content - Infrared absorption method after combustion in an induction furnace (routine method) (ISO 15350:2000) Aciers et fontes - Dosage du carbone et du soufre totaux - Mthode par absorption dans linfrarouge aprs combustion dans un fou

8、r induction (mthode pratique) (ISO 15350:2000) Stahl und Eisen - Bestimmung der Gesamtgehalte an Kohlenstoff und Schwefel - Infrarotabsorptionsverfahren nach Verbrennung in einem Induktionsofen (Standardverfahren) (ISO 15350:2000) This European Standard was approved by CEN on 18 March 2010. CEN memb

9、ers 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 standards may be obtained on applicati

10、on 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 translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has t

11、he same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Pola

12、nd, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by a

13、ny means reserved worldwide for CEN national Members. Ref. No. EN ISO 15350:2010: EContentsDIN EN ISO 15350:2010-08 EN ISO 15350:2010 (E) 2 Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle5 4 Reagents.5 5 Apparatus .6 6 Test method6 7 Sampling.7 8 Procedure .7 9 Expression of results 13

14、 10 Test report 14 Annex A (informative) Examples of diagram for analytical principles 16 Annex B (informative) Example calculation of a linearity check22 Annex C (informative) Additional information on international cooperative tests.23 Annex D (informative) Graphical representation of precision da

15、ta .27 ForewordDIN EN ISO 15350:2010-08 EN ISO 15350:2010 (E) 3 The text of ISO 15350:2000 has been prepared by Technical Committee ISO/TC 17 “Steel” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 15350:2010 by Technical Committee ECISS/TC 102 “Methods

16、of chemical analysis for iron 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 October 2010, and conflicting national standards shall be withdraw

17、n at the latest by October 2010. 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. According to the CEN/CENELEC Internal Regulations, th

18、e national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nether

19、lands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 15350:2000 has been approved by CEN as a EN ISO 15350:2010 without any modification. 1 ScopeThis International Standard specifies an infrared absorption

20、 method, after combustion in an induction furnace, forthe determination of the total carbon and sulfur content in steel and iron.The method is applicable to carbon contents of mass fraction between 0,005 % and 4,3 % and to sulfur contents ofmass fraction between 0,000 5 % and 0,33 %.This method is i

21、ntended to be used in normal production operations and is intended to meet all generally accepted,good laboratory practices of the type expected by recognized laboratory accreditation agencies. It usescommercially available equipment, is calibrated and calibration verified using steel and iron certi

22、fied referencematerials, and its performance is controlled using normal statistical process control (SPC) practices.This method can be used in the single element mode, i.e., determination of carbon and sulfur independently or inthe simultaneous mode, i.e., determination of carbon and sulfur concurre

23、ntly.2 Normative referencesThe following normative documents contain provisions which, through reference in this text, constitute provisions ofthis International Standard. For dated references, subsequent amendments to, or revisions of, any of thesepublications do not apply. However, parties to agre

24、ements based on this International Standard are encouraged toinvestigate the possibility of applying the most recent editions of the normative documents indicated below. Forundated references, the latest edition of the normative document referred to applies. Members of ISO and IECmaintain registers

25、of currently valid International Standards.ISO 437:1982, Steel and cast iron Determination of total carbon content Combustion gravimetric method.ISO 4934:1980, Steel and cast iron Determination of sulfur content Gravimetric method.ISO 4935:1989, Steel and iron Determination of sulfur content Infrare

26、d absorption method after combustion inan induction furnace.ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results Part 1: Generalprinciples and definitions.ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic methodfor th

27、e determination of repeatability and reproducibility of a standard measurement method.ISO 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediatemeasures of the precision of a standard measurement method.ISO 9556:1989, Steel and Iron Determination of to

28、tal carbon content Infrared absorption method aftercombustion in an induction furnace.ISO 10701:1994, Steel and iron Determination of sulfur content Methylene blue spectrophotometric method.DIN EN ISO 15350:2010-08 EN ISO 15350:2010 (E) 4 ISO 13902:1997, Steel and iron Determination of high sulfur c

29、ontent Infrared absorption method aftercombustion in an induction furnace.ISO 14284:1996, Steel and iron Sampling and preparation of samples for the determination of chemicalcomposition.3Principle3.1 CarbonThe carbon is converted to carbon monoxide and/or carbon dioxide by combustion in a stream of

30、oxygen.Measurement is by infrared absorption of the carbon monoxide and carbon dioxide carried by a current of oxygen.3.2 SulfurThe sulfur is converted to sulfur dioxide by combustion in a stream of oxygen. Measurement is by infraredabsorption of the sulfur dioxide carried by a current of oxygen.4 R

31、eagents4.1 Acetone, the residue after evaporation shall have a mass fraction less than 0,000 5 %.4.2 Cyclohexane, the residue after evaporation shall have a mass fraction less than 0,000 5 %.4.3 Inert ceramic, attapulques clay impregnated with sodium hydroxide and having particle sizes from 0,7 mmto

32、 1,2 mm for absorption of carbon dioxide.4.4 Pure iron, used as an accelerator, 0,4 mm to 0,8 mm size with carbon and sulfur contents with a massfraction of less than 0,001 % respectively.4.5 Magnesium perchlorate, reagent grade, having particle size from 0,7 mm to 1,2 mm for absorption ofmoisture.4

33、.6 Oxygen, ultra high purity (mass fraction minimum 99,5 % )An oxidation catalyst copper(II) oxide or platinum tube heated to 600 Gb0C followed by suitable carbon dioxide andwater absorbents shall be used when the presence of organic contaminants is suspected in the oxygen.4.7 Platinum or platinized

34、 silica, heated to 350 Gb0C for the conversion of carbon monoxide to carbon dioxide.4.8 Accelerator, copper, tungsten-tin or tungsten for carbon determination and tungsten for sulfur determination,0,4 mm to 0,8 mm size with carbon and sulfur contents of mass fraction less than 0,001 % and 0,000 5 %r

35、espectively.4.9 Cellulose cotton, for the collection of sulfur trioxide4.10 Steel and iron certified reference materials (CRMs), all reference materials used for calibration andcalibration verification shall be certified by internationally-recognized bodies and validated by adequateperformance on on

36、e or more national or international interlaboratory test programmes. Preference shall be given tomaterials that were certified using referee methods, e.g. ISO 437 and ISO 9556 for carbon, and ISO 4934,ISO 4935, ISO 10701 and ISO 13902 for sulfur, traceable to SI units as opposed to those based on ot

37、her certifiedreference materials.4.11 Steel and iron reference materials (RMs), those used for statistical process control of the method need notbe certified, but adequate homogeneity data shall be available, either from the certifying body or from the laboratorythat uses the material, in order to e

38、nsure the validity of the control data generated.DIN EN ISO 15350:2010-08 EN ISO 15350:2010 (E) 5 5 ApparatusOrdinary laboratory equipment plus the following shall be used.5.1 C and/or S determinator, consisting of an IR energy source, a separate measuring chamber and referencechamber, and a diaphra

39、gm acting as one plate of a parallel plate capacitor.5.2 Ceramic crucible, as specified by the manufacturer of the instrumentation used and capable of withstandingcombustion in an induction furnace without evolving carbon- and sulfur-containing chemicals so that achieving andmaintaining blank values

40、 within specification is possible.NOTE Carbon and sulfur contamination can usually be removed by igniting the crucibles in an electric furnace in air for notless than 40 min at 1 000 Gb0C or not less than 15 min at 1 350 Gb0C. After treatment, remove them from the heat, allow them to coolfor 2 min t

41、o 3 min on an appropriate clean heat-resistant tray and then store them in a desiccator.5.3 Crucible tongs, capable of handling recommended crucibles (5.2).6 Test methodThis test method is written for use with commercial analysers, equipped to carry out the included operationsautomatically and calib

42、rated using steels and irons of known carbon and sulfur contents.The analyser used will be satisfactory if it meets the criteria listed in clause 8.6.1 Infrared (IR) absorption for carbon Method AThe amount of carbon dioxide is measured by infrared absorption. Carbon dioxide (CO2) absorbs IR energy

43、at aprecise wavelength within the IR spectrum. Energy of this wavelength is absorbed as the gas passes through a cellbody in which the IR energy is transmitted. All other IR energy is prevented from reaching the detector by use of aprecise wavelength filter. Thus, the absorption of IR energy can onl

44、y be attributed to CO2and its concentration ismeasured as changes in energy at the detector. One cell is used as both a reference and a measuring chamber.Total carbon, as CO2, is monitored and measured over a period of time. See Figure A.1.6.2 Infrared (IR) absorption for carbon Method BDuring speci

45、men combustion, the flow of CO2with its oxygen gas carrier is routed through the measuring chamber(see 5.1) while oxygen alone passes through the reference chamber. Energy from the IR source passes throughboth chambers, simultaneously arriving at the diaphragm (capacitor plate). Part of the IR energ

46、y is absorbed by theCO2present in the measuring chamber while none is absorbed passing through the reference chamber. Thiscreates an IR energy imbalance reaching the diaphragm, thus distorting it. This distortion alters the fixedcapacitance creating an electric signal change that is amplified for me

47、asurement as CO2. Total carbon, as CO2,ismonitored and measured over a period of time. See Figure A.2.6.3 Infrared (IR) absorption for carbon Method C, closed loopThe combustion is performed in a closed loop, where CO and CO2are detected in the same infrared cell. Each gasis measured using a solid s

48、tate energy detector. Filters are used to pass the appropriate IR wavelength to eachdetector. In the absence of CO and CO2, the energy received by each detector is maximum. During combustion,the IR absorption properties of CO and CO2gases in the chamber cause a loss of energy; therefore a loss in si

49、gnalresults which is proportional to concentrations of each gas in the closed loop. Total carbon, as CO2plus CO, ismonitored and measured over a period of time. See Figure A.3.6.4 Infrared absorption for sulfur Method ASulfur dioxide (SO2) absorbs infrared (IR) energy at a precise wavelength within the IR spectrum. Energy of thiswavelength is absorbed as the gas passes through a cell body in which the IR energy is transmitted. All other IRenergy is prevented from reaching the detector by use of a precise wavelength filt