1、BRITISH STANDARD BS EN ISO 9556:2001 Incorporating Corrigendum No. 1 Steel and iron Determination of total carbon content Infrared absorption method after combustion in an induction furnace The European Standard EN ISO 9556:2001 has the status of a British Standard ICS 77.080 NO COPYING WITHOUT BSI
2、PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN ISO 9556:2001 This British Standard, having been prepared under the direction of the Engineering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 3 September 2001 BSI 13 Marc
3、h 2002 ISBN 0 580 38432 2 National foreword This British Standard is the official English language version of EN ISO 9556:2001. It is identical with ISO 9556:1989. It supersedes BS 6200-3.8.3:1990 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee ISE/18
4、, Sampling and analysis if iron and steel, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document ma
5、y be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British
6、Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals f
7、or change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, the ISO foreword p
8、age, pages 1 to 8, the Annex ZA page and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 13762 Corrigendum No. 1 13 March 2002 Incorporating Annex ZAEUROPEANSTANDARD NORMEEUROPENNE
9、 EUROPISCHENORM ENISO9556 June2001 ICS07.008.01 Englishversion SteelandironDeterminationoftotalcarboncontentInfrared absorptionmethodaftercombustioninaninductionfurnace (ISO9556:1989) AciersetfontesDosageducarbonetotalMthodepar absorptiondanslinfrarougeaprscombustiondansunfour induction(ISO9556:1989
10、) ThisEuropeanStandardwasapprovedbyCENon11May2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybe
11、obtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official version
12、s. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFR
13、NORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO9556:2001ECORRECTED20020102 Foreword ThetextoftheInternationalStandardfromTechnicalCommitteeISO/TC17“Steel“ofthe InternationalOrganizationf
14、orStandardization(ISO)hasbeentakenoverasaEuropean StandardbyTechnicalCommitteeECISS/TC20“Methodsofchemicalanalysisofferrous products“,thesecretariatofwhichisheldbySIS. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublication ofanidenticaltextorbyendorsement,atthelatestbyDecem
15、ber2001,andconflicting nationalstandardsshallbewithdrawnatthelatestbyDecember2001. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, CzechRepublic,Denmark,Finland,France,Germany,Greece,Icelan
16、d,Ireland,Italy, Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnited Kingdom. Endorsementnotice ThetextoftheInternationalStandardISO9556:1989hasbeenapprovedbyCENasa EuropeanStandardwithoutanymodification. NOTENormativereferencestoInternationalStandardsarelistedinannexZA(norma
17、tive). ENISO9556:2001INTERNATIONAL STANDARD IS0 9556 First edition 1989-07-15 Corrected and reprinted 1989-11-15 Steel and iron - Determination of total carbon content - Infrared absorption method after combustion in an induction furnace Aciers et fon tes - Dosage du carbone total - Mi induction par
18、 absorption dans Reference number IS0 9556 : 1989 (E) ENISO9556:2001Foreword IS0 (the lnternational Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technica
19、l 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, govern- mental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely w
20、ith the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the IS0 Council. They a
21、re approved in accordance with IS0 procedures requiring at least 75 % approval by the member bodies voting. International Standard IS0 9556 was prepared by Technical Committee lSO/TC 17, S tee/. Annexes A, B and C of this International Standard are for information only. ENISO9556:2001LANOITANRETNI D
22、RADNATS 0SI 6559 : 9891 )E( Steel and iron - Determination of total carbon content - Infrared absorption method after combustion in an induction furnace 1 Scope This International Standard specifies an infrared absorption method after combustion in an induction furnace for the deter- mination of the
23、 tota; carbon content in steel and iron. The method is applicable to carbon contents between 0,003 % (m/m) and 4,5 % (m/m). 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of pu
24、blication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encour- aged to investigate the possibility of applying the most recent editions of the standards listed below. Members of IEC and IS0 maintain regi
25、sters of currently valid International Standards. IS0 377: 1985, Wrought steel - Selection andpreparation of samples and test pieces. IS0 385-l : 1984, Laboratory glassware - Burettes - Part 7: General requirements. IS0 648 : 1977, Laboratory glassware - One-mark pipettes. IS0 1042 : 1983, Laborator
26、y glassware - One-mark volumetric flasks. IS0 5725 : 1986, Precision of test methods - Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests. 3 Principle Combustion of a test portion with accelerator at a high temperature in a high-frequency inductio
27、n furnace in a current of pure oxygen. Transformation of carbon into carbon dioxide and/or carbon monoxide. Measurement by infrared absorption of the carbon dioxide and/or carbon monoxide carried by a current of oxygen. 4 Reagents During the analysis, unless otherwise stated, use only reagents of re
28、cognized analytical grade and only distilled water or water of equivalent purity. 4.1 Water, free from carbon dioxide. Boil water for 30 min, cool to room temperature and bubble with oxygen (4.2) for 15 min. Prepare just before use. 4.2 Oxygen, 99,5 % (m/m) minimum. An oxidation catalyst copper oxid
29、e or platinum tube heated to a temperature above 450 OC must be used prior to a purify- ing unit (see annex C), when the presence of organic con- taminants is suspected in the oxygen. 4.3 Pure iron, of known low carbon content less than 0,001 0 % (m/m). 4.4 Suitable solvent, appropriate for washing
30、greasy or dirty test samples, for example, acetone. 4.5 Magnesium perchlorate Mg(Cl04)$, particle size : from 0,7 mm to I,2 mm. 4.6 Barium carbonate Dry barium carbonate (minimum assay : 99,5 %I at 105 OC to 110 OC for 3 h and cool in a desiccator before use. 4.7 Sodium carbonate Dry anhydrous sodiu
31、m carbonate (minimum assay: 99,9 %) at 285 OC for 2 h and cool in a desiccator before use. 4.8 Accelerator: copper, tungsten-tin mixture or tungsten of known low carbon content less than 0,001 0 % (m/m). 4.9 Sucrose, standard solution, corresponding to 25 g of C per Iitre. Weigh, to the nearest 1 mg
32、, 14,843 g of sucrose (C12HZO11) (analytical standards grade) previously dried at 100 OC to 105 OC for 2,5 h and cooled in a desiccator. ENISO9556:20010sI 6559 : 9891 )E Dissolve in about 100 ml of water (4.1), transfer to a 250 ml one-mark volumetric flask quantitatively, dilute to the mark with wa
33、ter (4.1) and mix. 1 ml of this standard solution contains 25 mg of C. 4.10 Sodium carbonate, standard solution, corresponding to 25 g of C per litre. Weigh, to the nearest 1 mg, 55,152 g of sodium carbonate (4.7), dissolve in about 200 ml of water (4.1), transfer to a 250 ml one-mark volumetric fla
34、sk quantitatively, dilute to the mark with water (4.1) and mix. 1 ml of this standard solution contains 25 mg of C. 4.11 I nert cera mic (attapulgus clay) impregnated sodium hydroxide, particle size : from 0,7 mm to 1,2 mm. with 5 Apparatus During the analysis, unless otherwise stated, use only ordi
35、nary laboratory apparatus. All volumetric glassware shall be class A, in accordance with IS0 385-1, IS0 648 or IS0 1042 as appropriate. The apparatus required for combustion in a high-frequency in- duction furnace and the subsequent infrared absorption measurement of the evolved carbon dioxide and/o
36、r carbon monoxide may be obtained commercially from a number of manufacturers. Follow the manufacturers instructions for the operation of the instrument. Features of commercial instruments are given in annex C. 5.1 Micropipette, 100 1, limit of error shall be less than 1 PI. 5.2 Tin capsule, about 6
37、 mm in diameter, 18 mm in height, 0,3 g in mass and approximately 0,4 ml in volume, of known low carbon content less than 0,001 0 % (m/m). 5.3 Ceramic crucible, capable of withstanding combustion in an induction furnace. Ignite crucibles in an electric furnace in air or in a current of oxygen for no
38、t less than 2 h at 1 100 OC and store in a desic- cator before use. NOTE - For the determination of low carbon contents it is advisable to ignite crucibles at 1 350 OC in a current of oxygen. 6 Sampling Carry out sampling in accordance with IS0 377 or appropriate national standards for iron, 7 Proce
39、dure SAFETY INSTRUCTIONS - The risks related to combus- tion analysis are mainly burns in pre-igniting the ceramic crucibles and in the fusions. Use crucible tongs at all times and suitable containers for the used crucibles. Nor- mal precautions for handling oxygen cylinders shall be taken. Oxygen f
40、rom the combustion process shall be removed effectively from the apparatus since a high con- centration of oxygen in a confined space can present a fire hazard. 7.1 General operating instructions Purify the oxygen supply using tubes packed with the inert ceramic (attapulgus clay) impregnated with so
41、dium hydroxide (4.11) and magnesium perchlorate (4.51, and maintain a quies- cent flow rate whilst on standby. Maintain a glass wool filter or a stainless steel net as a dust collector. Clean and change as necessary. The furnace chamber, pedestal post and filter trap shall be cleaned frequently to r
42、emove oxide build-up. Allow each item of equipment to stabilize for the time recom- mended by the equipment manufacturers when the main supply is switched on after being out of action for any length of time. After cleaning the furnace chamber and/or changing filters or after the equipment has been i
43、noperative for a period, stabilize the apparatus by burning several samples of similar type to the samples to be analysed prior to setting up for analysis. Flush oxygen through the apparatus and adjust the instrument controls to give a zero reading. If the instrument used provides a direct reading i
44、n percentage of carbon, adjust the instrument reading for each calibration range as follows. Select the certified reference material with a carbon content close to the maximum carbon content in the calibration series, measure the carbon content of the certified reference material in the manner speci
45、fied in 7.4. Adjust the reading of the instrument to the certified value. NOTE - This adjustment shall be made before the calibration as specified in 7.5. It cannot replace or correct the calibration. 7.2 Test portion Degrease the test sample by washing in a suitable solvent (4.4). Evaporate the las
46、t traces of the washing liquid by heating. Weigh, to the nearest 1 mg, approximately 1 g of the test sam- ple for carbon contents less than I,0 % (m/m) and approx- imately 0,5 g for carbon contents greater than 1,O % (m/m). NOTE - The mass of the test portion may be dependent on the type of instrume
47、nt used. 2 ENISO9556:20019891:6559OSI )E( 7.3 Blank test Prior to the determination, carry out the following blank tests in duplicate. Transfer the tin capsule (5.2) (see note I) to the ceramic cruci- ble (5.3), press the tin capsule lightly against the bottom of the crucible. Add the same quantity
48、of pure iron (4.3) as that of the test portion (7.2), and the same quantity of the accelerators (4.8) (see note 2) as will be added to the test portion. Treat the crucible and contents as specified in the second and third paragraphs of 7.4. Obtain the reading of the blank tests and convert it to milligrams of carbon by means of the calibration graph (7.5). The blank value is obtained by subtracting the mass of carbon in the pure iron used (4.3) from the mass of carbon in the blan
