DIN EN 10276-1-2000 Chemical analysis of ferrous materials - Determination of oxygen in steel and iron - Part 1 Sampling and preparation of steel samples for oxygen determination G.pdf

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1、DEUTSCHE NORM Auaust 2000 Determination of oxygen in steel and iron Part 1 : Sampling and preparation of steel samples for oxygen determination Enalish version of DIN EN 10276-1 DIN - EN 10276-1 ICs 77.040.30 Chemische Analyse von Eisenmetallen - Bestimmung des Sauerstoffgehalts von Stahl und Eisen

2、-Teil 1 : Herstellung und Vorbereitung der Stahlproben fr die Sauerstoff-Bestimmung European Standard EN 10276-1 : 2000 has the status of a DIN Standard. A comma is used as the decimal marker. National foreword This standard has been prepared by ECISS/TC 20. The responsible German body involved in i

3、ts preparation was the NormenausschussfisenundStah/(lron and Steel Standards Committee). EN comprises 7 pages. No pari of this standard may be reproduced without the prior permission of hiDeutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, s the exclusive right of

4、sale for German Standards (DIN-Normen). Ref. No. DIN EN 10276-1 : 2000-0 English price group 06 Sales No. 1106 o1 .o1 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 10276-1 May 2000 ICs 77.040.30 English version Chemical analysis of ferrous materials Part 1 : Sampling and preparation of steel

5、samples for oxygen determination Determination of oxygen in steel and iron Analyse chimique des matriaux sidrurgiques - Dosage de loxygne dans les aciers et les fontes - Partie 1 : Echantillonnage et prparation des chantillons en acier pour dosage de loxygne Bestimmung Chemische Analyse von Eisen- m

6、etallen - Bestimmung des Sauer- stoffgehalts von Stahl und Eisen - Teil 1 : Herstellung und Vorbereitung der Stahlproben fr die Sauerstoff- This European Standard was approved by CEN on 2000-04-22. CEN members are bound to comply with the CENKENELEC Internal Regulations which stipulate the condition

7、s for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national stand- ards may be obtained on application to the Central Secretariat or to any CEN member. The European Standards exist in three off

8、icial 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 Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria,

9、 Belgium, the Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, and the United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normun

10、g Central Secretariat: rue de Stassart 36, B-1050 Brussels O 2000. CEN - All rights of exploitation in any form and by any means reserved worldwide for CEN national members. Ref. No. EN 10276-1 : 2000 E Page 2 EN 10276-1 : 2000 Contents Foreword . . . . . . , , . . . . . . . . . . . . . . . . . . .

11、. , . . . . , . , 2 1 Scope 3 2 Normative reference ._ 3 3 Principle .,. 3 4 Reagents . 3 5 Apparatus 3 6 Sampling . 4 7 Sample preparation . 4 Foreword This European Standard has been prepared by Technical Committee ECISSTTC 20 “Methods of chemical analysis of ferrous products”, the secretariat of

12、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 November 2000, and conflicting national standards shall be withdrawn at the latest by November 2000. According to the CENKENEL

13、EC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Swit

14、zerland and the United Kingdom. Page 3 EN 10276-1 : 2000 1 Scope This European Standard specifies two methods for the preparation of steel samples for oxygen determination. Both methods are suitable for preparing samples for the determination of oxygen content, especially for oxygen contents 0,0050

15、YO. This standard is applicable to steels having a hardness of c 400 HBW 10/3000. 2 Normative reference This European Standard incorporates by dated or undated reference provisions from other publications. These normative references are cited at the appropriate places in the text and the publication

16、s are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendmen

17、ts). IS0 14284 Steel and iron - Sampling and preparation of samples for the determination of chemical composition 3 Principle Samples for oxygen determination are machined to a suitable shape and size within the restrictions imposed by the instrument used. In order to ensure that the surface has the

18、 minimum possible oxygen content, samples for analysis are prepared either by punching (method A) or by turning (method B). 4 4.1 4.2 5 5.1 5.1.1 5.1.2 5.1.3 5.2 5.2.1 Reagents Organic oxygen free hydro carbon solvent e.g. n-hexane; (boiling-point range: 68 OC to 69 OC) Argon or nitrogen Apparatus M

19、ethods A and 6 Mechanical steel saw Tweezers Receptacles for storing the test samples e.g. glass tubes about 2,5 cm long and about 1 cm in diameter with stopperskaps. Method A: Punch: suitable for punching out samples in the manner described in 7.1.4. Purging by argon or nitrogen ensures minimum pos

20、sible contact of the samples with atmospheric oxygen. This is illustrated in figure 1. 5.2.2 5.2.3 5.3 Method B: 5.3.1 5.3.2 Flat bed linisher for linishing the steel sample. Electrical hand drill and rotary file, with rotation speed exceeding 30 O00 rev/min. Lathe for turning steel samples at speed

21、s of 250 rev/min to 1 200 rev/min. Hand saw: the saw blade shall be free from grease or paint. Page 4 EN 10276-1 : 2000 5.3.3 Filing block made of stainless steel which holds the samples firm during filing of the end-faces (figure 2). 5.3.4 Hand files: cut no. 4. 5.3.5 Metal wire brush with strong b

22、ristles about 2 cm long. 6 Sampling Sampling for preparation of the analytical samples shall proceed in accordance with IS0 14284. The distribution of oxygen within the product is dependent on the manufacturing process. The result of the oxygen determination will therefore depend on the sample posit

23、ion. This has to be agreed if it is not specified in the product standard. 7 7.1 7.1.1 7.1.2 7.1.3 7.1.4 7.1.5 7.2 7.2.1 Sample preparation Method A Punching Saw off slices 3 mm to 4 mm thick from the sample piece using a mechanical saw (5.1.1). The number shall be as required by the method. NOTE: F

24、igures 3 and 4 give examples of the different procedures for different sample shapes. Use a flat bed linisher (5.2.2) with 60 grade silicon carbide paper so that the sample slices are ground flat on both sides removing most of the oxide layer. Hold the sample with a magnetic holding device during gr

25、inding. Remove thoroughly any oxides remaining on the surface with a rotary file under a flow of argon or nitrogen (5.2.3). The condition of the surface after preparation shall be smooth, bright and free from burrs and irregularities. Avoid significant heating of the sample in order to prevent oxida

26、tion of the surface after removal from inert atmosphere. After treatment, handle the samples with tweezers only. Do not touch the samples by hand. NOTE: During milling and all subsequent preparations, take care to ensure that the tools and objects coming into contact with the sample are free from ox

27、ygen containing contaminants. The test samples should usually have a mass of approximately 1 g. The mass of the sample depends on the method of oxygen determination. Prepare the samples with a punch (52.1). A punch of 4 to 6 mm diameter is normally suitable for this purpose. During the punching oper

28、ation purge the receptacle into which the sample is collected, with argon or nitrogen (4.2) (figure 1) Keep the test samples in a glass receptacle (5.1.3). Samples should be analysed as soon as possible on the same day as preparation. Immediately before analysis, wash the test samples in organic sol

29、vent (4.1) and dry them in air or under vacuum free from backgassing. NOTE: Problems with microcracks have been encountered in the determination of low levels of carbon ( l0ppm). There may be similar contamination problems in the determination of oxygen. Method B Turning Take rectangular pieces abou

30、t 100 mm long with a cross section of about 10 mm x 10 mm from the sample piece with a mechanical saw. Figures 3 and 4 give examples of the various procedures for different shapes of samples. If rods, wire or forged pieces of about 10 mm diameter are available, it is only necessary to cut off one pi

31、ece about 100 mm in length. Page 5 EN 10276-1 : 2000 7.2.2 The test samples should usually have a mass of approximately 1 g. The mass of the sample depends on the method of oxygen determination. Prepare these samples by turning the pieces on a lathe (5.3.1). For this purpose, turn down the sample ob

32、tained in accordance with 7.2.1, to about 7 mm diameter at a speed of about 1 O00 rev/min. Subsequent turning down to 6 mm diameter shall be at a speed of 250 rev/rnin with a feed of about 0,2 mm/rev. After turning, file the surface with a fine file (5.3.4) with the lathe still running until the sam

33、ple is smooth and bright. Avoid significant heating of the sample in order to prevent oxidation of the surface. As an altemative to slow-speed turning, reduce the diameter from 7 mm to 6 mm using a speed of between 800 rev/min to 1 O00 rev/min and a feed of between 0,l-0,15 mm/rev. In this case, the

34、 cylindrical surface is smooth enough to dispense with the filing operation. NOTE: Use no cooling lubricant during turning down from 7 mm to 6mm Take care also during the subsequent stages in preparation to ensure that any objects coming into contact with the sample are free from oxygen containing c

35、ontaminants. 7.2.3 Using the hand saw (5.3.2), saw off the end of the sample which is not used for analysis. Clean the accessible end face of the clamped sample by filing. Then, saw off a test sample 4 mm to 5 mm long for analysis. Handle the sample with tweezers only. Do not touch samples by hand.

36、Use the tweezers for all manipulations. File carefully the unfiled end face of the sample in a filing block (figure 2) or in another similar holding device. Remove carefully any adhering dust with a small brush (5.3.5). Keep the test samples in a glass receptacle (5.1.3). These shall be analysed as

37、soon as possible on the same day as they were prepared. Immediately before analysis, wash the samples in organic solvent (4.1) and dry them in air or under vacuum free from backgassing. V/ Sample holder Argon (nitrogen) _3. inlet Sample slice or disc - Glass receptacle Figure 1 - Punch for making sa

38、mples for oxygen analysis Page 6 EN 10276-1 : 2000 Sample I 7 oxygen analysis rn! / 150 I- Figure 2 - Filing block Method A Rolling Method B 1 Sample piece 2 A and 2 B Sections sawn out of the sample piece 3 Sawn-out sample slice; the shaded circles denote the positions at which the samples can be p

39、unched out. 4 Produced from 28 by turning. 5 Produced by turning, from which the test samples (shaded zones) are sawn. Figure 3 - Example of production of test samples from a sample piece Page 7 EN 10276-1 : 2000 Method B 1 2 Sample piece Sample slice/disc sawn off. The shaded circles denote the positions at which the samples can be punched out. Bar sawn out of the sample piece Bar produced from (3) by turning Bar produced by turning down from which the test samples (indicated by shading) can be sawn. Figure 4 - Example of production of test samples from a sample piece