BS EN 10036-1991 Chemical analysis of ferrous materials - Determination of total carbon in steels and irons - Gravimetric method after combustion in a stream of oxygen《黑色金属材料的化学分析 .pdf

1、BRITISH STANDARD BS EN 10036:1991 Chemical analysis of ferrous materials Determination of totalcarbon in steelsandirons Gravimetric method after combustion in a stream of oxygen This European Standard EN10036:1989 has the status of a British StandardBSEN10036:1991 This British Standard was published

2、 under the authority ofthe Board of BSI and comesintoeffect on 31January1991 BSI12-1999 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft for approval 83/70400 ISBN 0 580 19305 5 Cooperating organizations The European Committee for Standardization, un

3、der whose supervision this European Standard was prepared, comprises the national standards organizations of the following Western European countries. Austria Oesterreichisches Normungsinstitut Belgium Institut belge de normalisation Denmark Dansk Standardiseringsraad Finland Suomen Standardisoimisl

4、iito, r.y. France Association franaise de normalisation Germany Deutsches Institut fr Normung e.V. Greece Hellenic Organization for Standardization Iceland Technological Institute of Iceland Ireland National Standards Authority of Ireland Italy Ente Nazionale Italiano di Unificazione Luxemburg Inspe

5、ction du Travail et des Mines Netherlands Nederlands Normalisatie-instituut Norway Norges Standardiseringsforbund Portugal Instituto Portugus da Qualidade Spain Asociacin Espaola de Normalizacin y Certificacin Sweden Standardiseringskommissionen i Sverige Switzerland Association suisse de normalisat

6、ion United Kingdom British Standards Institution Amendments issued since publication Amd. No. Date of issue CommentsBSEN10036:1991 BSI 12-1999 i Contents Page Cooperating organizations Inside front cover National foreword ii Brief history 2 Text of EN 10036 3 National appendix NA Inside back coverBS

7、EN10036:1991 ii BSI 12-1999 National foreword This British Standard has been prepared under the direction of the Iron and Steel Standards Policy Committee. It is the English language version of EN10036:1989 “Chemical analysis of ferrous materials. Determination of total carbon in steels and irons. G

8、ravimetric method after combustion in a stream of oxygen”, published by the European Committee for Standardization (CEN). It supersedes BS6200-3.8.1:1985, which is withdrawn. Attention is drawn to the fact that this standard specifies the use of soda asbestos. In view of the hazardous nature of asbe

9、stos, a suitable alternative reagent, for example an inert ceramic impregnated with sodium hydroxide, should be used instead. A proposal to amend the text of the European Standard has been submitted to the CEN Central Secretariat. A further method for the determination of carbon in ferrous materials

10、 has been published as BS6200-3.8.3. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summ

11、ary of pages This document comprises a front cover, an inside front cover, pagesi andii, theEN title page, pages2 to6, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on

12、 the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN10036 January1989 UDC669.1:542.26:543.21 Key words: Iron- and steel products; steels; cast iron; chemical analysis; determination of content; carbon; gravimetric analysis; combustion analysis English version Chemical analysi

13、s of ferrous materials Determination of total carbon in steels and irons Gravimetric method aftercombustion in a stream of oxygen Analyse chimique des matriaux sidrurgiquesDosage du carbone total dansles aciers et les fontesMthode gravimtrique aprs combustion dans un courant doxygne Chemische Analys

14、e von Eisen- und Stahlwerk- stoffenErmittlung des Gesamtkohlenstoffgehalts von Stahl und RoheisenGewichtsanalytische Ermittlung nach Verbrennung im Sauerstoffstrom This European Standard was accepted by CEN on15 January1989. CEN members are bound to comply with the requirements of the CEN/CENELEC Ru

15、les 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 application to the CEN Central Secretariat or to any CEN member. This E

16、uropean Standard exists in the 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 CEN Central Secretariat has the same status as the official versions. CEN members are the nat

17、ional standards organizations of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxemburg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee

18、 fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels CEN1989 Copyright reserved to all CEN members Ref. No. EN10036:1989 EEN10036:1989 BSI 12-1999 2 Brief history This European Standard takes over the content of EURONORM36-83 “Chemical analysis of ferrous materialsDetermination of to

19、tal carbon in steels and ironsGravimetric method after combustion in a stream of oxygen”, prepared by ECISS/TC20 “Methods of chemical analysis”, the Secretariat of which is allocated to the Dansk Standardiseringsrad (DS). It has been submitted to the CEN Formal Vote following the decision of the Coo

20、rdinating Commission (COCOR) of the European Committeefor Iron and Steel Standardization on1987-11-24/25. It has been adopted and ratified by CEN BT on1988-11-05. According to the Common CEN/CENELEC Rules, following countries are bound to implement this European Standard: Austria, Belgium, Denmark,

21、Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxemburg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. Note in clauses1 and9 EURONORM shall read EUROPEAN STANDARD. Contents Page Brief history 2 1 Scope and field of application 3 2 Reference 3 3 Principle 3

22、 4 Reagents 3 5 Apparatus 3 6 Sampling 4 7 Procedure 4 7.1 Test portion 4 7.2 Blank test 4 7.3 Determination 5 8 Expression of results 5 9 Test report 5 Figure 1 Apparatus for the gravimetric determination of the total carbon after combustion in a stream of oxygen 6 Figure 2 Absorption bulb 6EN10036

23、:1989 BSI 12-1999 3 1 Scope and field of application This EURONORM specifies a gravimetric method for the determination of total carbon in steels and irons after combustion in a stream of oxygen. The method is applicable to carbon contents equal to or greater then0.1% (m/m). 2 Reference EURONORM18Se

24、lection and preparation of samples and test pieces for steel and iron and steel products. 3 Principle Combustion of a test portion in a stream of oxygen in a high temperature furnace(1200-14430 C), with the addition of a fluxing agent to assist combustion. Absorption of the evolved carbon dioxide in

25、 soda asbestos contained in a weighed absorption bulb. Calculation of the carbon content from the increase in mass of the absorption bulb. 4 Reagents During the analysis, use only reagents of recognized analytical quality. 4.1 Oxygen, cylinder oxygen, of at least99%purity. 4.2 Magnesium perchlorate

26、(Anhydrone) as a drying agent. 1) 4.3 Fluxes: lead oxide, copper (II) oxide, tin filings:high purity iron chips of certified very low carbon content. 4.4 Copper (II) oxide, granulated. 4.5 Soda asbestos, in granules of approximately2mm diameter. Avoid contact with air. Handling of this reagent shoul

27、d take place under a fume hood with sufficient suction to avoid inhalation of asbestos dust by the operator. 4.6 Sulphuric acid, 1.84g/ml approximately.(18mol/l approximately). 4.7 Chromic-sulphuric acid; Saturate a sulphuric acid solution, 1.23g/ml approximately(4mol/l approximately) with chromic a

28、cid anhydride(CrO 3 ). The solution remains effective only as long as it retains its red colour. Sulphuric acid solution 1.23 approximately, is prepared by diluting sulphuric acid =1.84g/ml.1+4 with water. 5 Apparatus The apparatus consists of three parts: The first partincludes the oxygen cylinder

29、and the oxygen-purifier, the second part comprises the furnace and combustion tube and the third part comprises the vessels for purification and absorption of the carbon dioxide produced by combustion of the carbon in the analysis sample. The three parts, which are interconnected by tubing and herme

30、tically sealed stoppers, are depicted inFigure 1. 1) Contact with organic substances should be avoided because of the potential hazard of an explosion. Figure 1 A Oxygen cylinder(4.1) with a pressure regulating valve. B Mercury valve. C Furnace with non-porous porcelain tube, heated to400 C, contain

31、ing granules of copper (II) oxide(4.4). D U tube containing magnesium perchlorate(4.2) and soda asbestos(4.5) separated by glass wool for drying and purification of oxygen (diameter of the tubes is25mm, height approximately100mm with connection). The U tube must be packed in such a manner that the o

32、xygen passes first through the soda asbestos and afterwards through the magnesium perchlorate. E Electric resistance furnace, capable of raising the temperature of the combustion tube to1400 C. F Thermocouple for temperature measurement. The point of the thermocouple protected by its own sheath is p

33、laced near the external surface of the combustion tube. It is recommended that the difference between the external and the internal temperature of the tube should be checked. G Refractory combustion tube which is not porous at the test temperature, having an internal diameter of20 to30mm and a lengt

34、h of at least600mm so that the ends of the tube remain cool during the combustion. The tube should extend beyond each end of the furnace by not less than150mm.EN10036:1989 4 BSI 12-1999 6 Sampling Sampling shall be carried out in accordance with EURONORM18. The sample as prepared for analysis shall

35、be in the form of very short chips having a thickness not exceeding a few tenths of a millimetre. For white cast irons the analysis sample must be fine enough to pass through a sieve of0.18mm mesh size. For grey cast irons the test piece shall be cut into plates2mm thick and broken up with pliers to

36、 avoid the possibility of errors arising from the segregation of graphite. 7 Procedure Alter checking the leak-tightness of the apparatusand having attained a temperature of1200-1400 C in the combustion zone of the furnace (use highest temperature for the more highly alloyed steels), allow the oxyge

37、n(4.1) to flow into the apparatus for10 to15minutes, at a rate of300 to500mlper minute depending on the diameter of the tube used. Next disconnect the absorption bulbs and close the taps to avoid contact with ambient air. Weigh them after10minutes at ambient temperature and then reconnect them to th

38、e apparatus. 7.1 Test portion Weigh the masses (m) given below as a function of presumed carbon content to the nearest0.001g remaining within the tolerance of1096 of the specified mass: a) content from0.1%to1%m approximately2g: b) content above1%, m approximately1g. Transfer the weighed test portion

39、 to the calcined refractory boat. Add to the sample1 to2g of carefully weighed flux(4.3). 7.2 Blank test Determine the blank value of the apparatus, boat and flux by combustion of the boat containing the prescribed quantity of flux(4.3) exactly in accordance with the conditions specified for the ana

40、lysis(7.3) and record the increase in mass (massm 0 ) of the absorption bulb. Where there is any doubt about the purity of the boat, this should be verified by the combustion in the boat of the exact amount of flux used in the analysis, together with1g of high purity iron of certified very low carbo

41、n content(4.3). In this case, the blank value (mass m 0 ) is obtained after correcting for the certified carbon content of the high purity iron. The leak-tightness of the apparatus and the effectiveness of the purification system can be checked without submitting materials and fluxes to combustion.

42、H Refractory boat with eyelet (length80 to100mm, width12 to14mm, height8 to9mm) calcined in a current of oxygen under the working conditions. I,I Small, porous refractory cylinders for protecting the end stoppers of the combustion tube against the heat. For subsequently cooling the tube, its ends ca

43、n be enclosed by water-circulating lead or copper coils. L Glass bulb tube filled with quartz wool to trap the dust carried along by the gas flow. M Wash bottle containing the chromic-sulphuric acid(4.7). M Drier containing the magnesium perchlorate(4.2). N Contact furnace with non-porous porcelain

44、tube, heated to400 containing copper (II) oxide granules(4.4), in order to ensure complete oxidation to carbon dioxide. O,O Weighed absorption bulbs with turn off taps, for the absorption of the carbon dioxide, containing soda asbestos(4.5) and a layer(10-20mm) of magnesium perchlorate(4.2) for reta

45、ining the water formed during the absorption of the carbon dioxide. The total mass of each absorption bulb, ready for use, should not exceed100g (seeFigure 2). O Unweighed absorption bulb, facing the opposite way to O and O. P Bottle of sulphuric acid(4.6) for the protection of the absorption bulbs

46、against the outside atmosphere and also for monitoring the rate of the oxygen flow.EN10036:1989 BSI 12-1999 5 7.3 Determination Cut off the oxygen flow, then open the combustion tube at the end where the oxygen enters and introduce the boat with the sample into the middle of the heated zone of the t

47、ube by means of a rigid nickel rod. Close the tube immediately and after one minute allow an oxygen flow to pass through at a rate of300 to500ml per minute depending on the diameter of the tube used. Combustion should be complete after approximately2 minutes but continue the oxygen flow for a furthe

48、r15 to20 minutes to ensure the complete expulsion of the carbon dioxide from the combustion tube and the purification bulbs. Cut off the oxygen flow, close the taps of the weighed absorption bulbs and remove the refractory boat from the combustion tube. Check whether the combustion has been properly

49、 carried out by examining the fused mass in the boat withdrawn from the furnace. Complete combustion is indicated by a totally fused mass in which no traces of the original sample can be recognized. Disconnect the absorption bulbs and after10minutes weigh them at ambient temperature. The increase in mass represents the carbon dioxide absorbed (mass m 1 ). 8 Expression of results The percentage by mass of carbon (C) is given by the expression: 9 Test report The test report shall contain the following particulars: a) the method