1、BRITISH STANDARDBS 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)ICS 77.080.01NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWNational forewordThis British St
2、andard is the UK implementation of EN ISO 15350:2010. It is identical to ISO 15350:2000. It supersedes BS ISO 15350:2001 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee ISE/18, Sampling and analysis of iron and steel.A list of organizations represented
3、 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.Compliance with a British Standard cannot confer immunity from legal obligations.BS EN ISO 15350:2
4、010This British Standard, having been prepared under the direction of the Engineering Sector Committee, was published under the authority of the Standards Committee and comes into effect on15 June 2001 BSI 2010Amendments/corrigenda issued since publicationDate Comments 30 June 2010 This corrigendum
5、renumbers BS ISO 15350:2001 as BS EN ISO 15350:2010 ISBN 978 0 580 69259 8EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15350 April 2010 ICS 77.080.01 English Version Steel and iron - Determination of total carbon and sulfur content - Infrared absorption method after combustion in an indu
6、ction 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 four induction (mthode pratique) (ISO 15350:2000) Stahl und Eisen - Bestimmung der Gesamtgehalte an Kohlenstoff und Schwefel - Inf
7、rarotabsorptionsverfahren nach Verbrennung in einem Induktionsofen (Standardverfahren) (ISO 15350:2000) This European Standard was approved by CEN on 18 March 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Stand
8、ard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards 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
9、, 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 the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia,
10、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 United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATIO
11、N 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 any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15350:2010: EForeword The text of ISO 15350:2000 has been
12、 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 of chemical analysis for iron and steel” the secretariat of which is held by SIS. This European Sta
13、ndard 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 withdrawn at the latest by October 2010. Attention is drawn to the possibility that some of the elements of
14、 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, the national standards organizations of the following countries are bound to implement this European
15、Standard: Austria, Belgium, Bulgaria, Croatia, 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 Un
16、ited Kingdom. Endorsement notice The text of ISO 15350:2000 has been approved by CEN as a EN ISO 15350:2010 without any modification. BS EN ISO 15350:2010EN ISO 15350:2010 (E)iiiContents Page1 Scope 12 Normative references 13 Principle24 Reagents.25 Apparatus .36 Test method37 Sampling.48 Procedure
17、.49 Expression of results 1010 Test report 11Annex A (informative) Examples of diagram for analytical principles 13Annex B (informative) Example calculation of a linearity check19Annex C (informative) Additional information on international cooperative tests.20Annex D (informative) Graphical represe
18、ntation of precision data .24BS EN ISO 15350:2010EN ISO 15350:2010 (E)This page deliberately set blankINTERNATIONAL STANDARD1Steel and iron Determination of total carbon and sulfurcontent Infrared absorption method after combustion in aninduction furnace (routine method)1 ScopeThis International Sta
19、ndard specifies an infrared absorption 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
20、 0,000 5 % and 0,33 %.This method is intended 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 calibrati
21、on verified using steel and iron certified 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., deter
22、mination of carbon and sulfur concurrently.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
23、do not apply. However, parties to agreements 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. Mem
24、bers of ISO and IECmaintain registers 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 D
25、etermination of sulfur content Infrared 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
26、and results Part 2: Basic methodfor the 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 9556:19
27、89, Steel and Iron Determination of total carbon content Infrared absorption method aftercombustion in an induction furnace.ISO 10701:1994, Steel and iron Determination of sulfur content Methylene blue spectrophotometric method.BS EN ISO 15350:2010EN ISO 15350:2010 (E)2 ISO 13902:1997, Steel and iro
28、n Determination of high sulfur content 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 dioxi
29、de by combustion in a stream of 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 ca
30、rried by a current of oxygen.4 Reagents4.1 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 hav
31、ing particle sizes from 0,7 mmto 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,
32、2 mm for absorption ofmoisture.4.6 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 o
33、xygen.4.7 Platinum or platinized 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
34、less than 0,001 % and 0,000 5 %respectively.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 valida
35、ted by adequateperformance on one 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
36、 as opposed to those based on other 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
37、uses the material, in order to ensure the validity of the control data generated.BS EN ISO 15350:2010EN ISO 15350:2010 (E)35 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 refere
38、ncechamber, and a diaphragm 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 an
39、dmaintaining blank values 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, allo
40、w them to coolfor 2 min to 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 operatio
41、nsautomatically and calibrated 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
42、 (CO2) absorbs IR energy 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 absorp
43、tion of IR energy can only 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 ca
44、rbon Method BDuring specimen 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 pla
45、te). Part of the IR energy 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
46、 that is amplified for measurement 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
47、 measured using a solid state 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 energ
48、y; therefore a loss in signalresults 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 p
49、recise 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 filter. Therefore, the absorption ofBS EN ISO 15350:2010EN ISO 15350:2010 (E)4 IR energy can only be attributed to SO2and its concentration is measured as changes in energy at the detector.One cell is used as both a reference and a measure chamber. Total sulfur, as SO2, is monitor
