1、Chemical analysis of ferrous materials - Determination of oxygen in steel and iron - Part 1: Sampling and preparation of steel samples for oxygen determination The European Standard EN 1027 - present to the responsible European committee any enquiries on the interpretation, or proposais for change,
2、and keep the UK interests informed; - monitor related intemational and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement intemational or Europe
3、an publications referred to in this document may 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 Elecbonic Catalogue. A British Standad does not purport to include ad the necessary
4、 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. Summary of pages This document comprises a front cover, an inside front cover, the EN titie page, pages 2
5、 to 10, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. This British Standard, having been prepared under the direction of the Engineering Sedor Committee, was published under the authority of the Standards Commi
6、ttee and comes into effect on 15 August 2000 Amendments issued since publication Comments Amd*No* ID* Q BSI 082000 ISBN O 580 34977 2 STDmBSI BS EN 1027b-L-ENGL 2000 Lb24bb9 0862850 39T EUROPEAN STANDARD EN 10276-1 NORME EUROPENNE EUROPISCHE NORM May 2000 ICs 77.040.30 English version Chemical analy
7、sis of ferrous materials - Determination of oxygen in steel and iron - Part 1: Sampling and preparation of steel samples for oxygen determination Analyse chimique des matriaux sidrurgiques - Dosage de loxygne dans les aciers et les fontes - Partie 1: Echantillonnage et prparation des chantillons en
8、acier pour dosage de loxygne Chemische Analyse von Eisenmetallen - Bestimmung des Sauerstoffgehalts von Stahl und Eisen -Teil 1: Herstellung und Vorbereitung der Stahlproben fr die Sauerstoff- Bestimmung This European Standard was approved by CEN on 22 April 2000. CEN members are bound to comply wit
9、h the CENICENELEC 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 sich national standards may be obtained on application to the Central Secretari
10、at or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by tmslation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as he official ver
11、sions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMIlTEE FOR STANDARDIZATION COMIT EUROPEN
12、 DE NORMALISATION EUROPISCHES KOMITEE FOR NORMUNG Central Secretariat: rue de Stassart. 36 8-1050 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 3 I Scope 4
13、2 Normative reference . 4 3 Principle 4 4 Reagents . 4 5 Apparatus 4 6 Sampling . 5 7 Sample preparation . 5 O BSI 08-2000 STD-BSI BS EN 10276-1-ENGL 2000 = Lb24bb 08b2852 162 m Page 3 EN 10276-1 2000 Foreword This European Standard has been prepared by Technical Committee ECISSTTC 20, Methods of ch
14、emical analysis of ferrous products, 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 November 2000, and conflicting national standards shall be withdrawn a
15、t the latest by November 2000. According to the CENEENELEC 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, Luxemb
16、ourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. O BSI 08-2000 Page 4 EN 10276-1 :2000 I 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 de
17、termination of oxygen content, especially for oxygen contents c 0,005 O %. This standard is applicable to steels having a hardness of 400 HBW 1013000. 2 Normative reference This European Standard incorporates by dated or undated reference provisions from other publications. These normative reference
18、s are cited at the appropriate places in the text and the publications 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 late
19、st edition of the publication referred to applies (including amendments). 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 impos
20、ed by the instrument used. In order to ensure that the surface has the 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 hydrocarbon solvent, e.g. n-hexan
21、e (boiling-point range: 68C to 69 OC). Argon or nitrogen. Apparatus Methods A and B 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 stopperdcaps. Method A: Punch: suitable for punching out samples in the man
22、ner described in 7.1.4. Purging by argon or nitrogen ensures minimum possible contact of the samples with atmospheric oxygen. This is illustrated in Figure 1. 5.2.2 5.2.3 Flat bed finisher for finishing the steel sample. Electrical hand drill and rotary file, with rotation speed exceeding 30 O00 rev
23、/min. O BSI 08-2000 STD-BSI BS EN L027b-L-ENGL 2000 Lb24bb9 Dab2854 T35 Page 5 EN 10276-1 12000 5.3 Method B: 5.3.1 Lathe for turning steel samples at speeds of 250 revlmin to 1 200 revlmin. 5.3.2 Hand saw: the saw blade shall be free from grease or paint. 5.3.3 Filing block made of stainless steel
24、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 bristles about 2 cm long. 6 Sampling Sampling for preparation of the analytical samples shall proceed in accordance with IS0 14284. The distribution of oxygen withi
25、n the product is dependent on the manufacturing process. The result of the oxygen determination will therefore depend on the sample position. This has to be agreed if it is not specified in the product standard. 7 7.1 7.1 .I 7.1.2 7.1.3 7.1.4 7.1.5 Sample preparation Method A Punching Saw off slices
26、 3 mm to 4 mm thick from the sample piece using a mechanical saw (5.1 .I). The number shall be as required by the method. NOTE: Figures 3 and 4 give examples of the different procedures for different sample shapes. Use a flat bed finisher (5.2.2) with 60 grade silicon carbide paper so that the sampl
27、e slices are ground flat on both sides removing most of the oxide layer. Hold the sample with a magnetic holding device during grinding. Remove thoroughly any oxides remaining on the surface with a rotary file under a flow of argon or nitrogen (52.3). The condition of the surface after preparation s
28、hall be smooth, bright and free from burrs and irregularities. Avoid significant heating of the sample in order to prevent oxidation 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
29、all subsequent preparations, take care to ensure that the tools and objects coming into contact with the sample are free from oxygen 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. Prepar
30、e the samples with a punch (5.2.1). A punch of 4 to 6 mm diameter is normally suitable for this purpose. During the punching operation purge the receptacle into which the sample is collected, with argon or nitrogen (4.2) (Figure I). Keep the test samples in a glass receptacle (5.1.3). Samples should
31、 be analyzed as soon as possible on the same day as preparation. Immediately before analysis, wash the test samples in organic solvent (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 (
32、 I O ppm). There may be similar contamination problems in the determination of oxygen. O BSI 08-2000 STD=BSI BS EN 1027b-1-ENGL 2000 bb24bb OBb255 971 m Page 6 EN 10276-1 :2000 7.2 Method B Turning 7.2.1 Take rectangular pieces about 100 mm long with a cross section of about 10 mm x 10 mm from the s
33、ample 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 1 O mm diameter are available, it is only necessary to cut off one piece about 100 mm in length. 7.2.2 The test samples should usually h
34、ave 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 obtained in accordance with 7.2.1, to about 7 mm diameter at a speed of about I O00 rev/min. S
35、ubsequent turning down to 6 mm diameter shall be at a speed of 250 rev/min 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 sample is smooth and bright. Avoid significant heating of the sample in order to prevent oxidati
36、on of the surface. As an alternative 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 to 0,15 mmhev. In this case, the cylindrical surface is smooth enough to dispense with the filing operation. NOTE: Use no
37、cooling lubricant during turning down from 7 mm to 6 mm. 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 contaminants. 7.2.3 Using the hand saw (5.3.2), saw off the end of the sample which is no
38、t 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. Use the tweezers for all manipulations. File carefully the unfiled end face of the sampl
39、e 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 analyzed as soon as possible on the same day as they were prepared. Immediately before analysis, was
40、h the samples in organic solvent (4.1) and dry them in air or under vacuum free from backgassing. O BSI 08-2000 STDmBSI BS EN 10276-1-ENGL 2000 1624669 OB62856 808 W Page 7 EN 10276-1 :2000 Sa ho Argon (nitrogen) inlet Sciiple si or disc Glass Figure 1 - Punch for making samples for oxygen analysis
41、ice receptoc le O BSI 08-2000 Sample /- oxygen analysis Figure 2 - Filing block Q BSI 08-2000 STD.BS1 BS EN L027b-1-ENGL 2000 Lb24bb9 0862858 680 Page 9 EN 10276-1 12000 Method A rolling direction Method B 5 1. Sample piece. 2A and 2B. 3. Sections sawn out of the sample piece. Sawn-out sample slice;
42、 the shaded circle- denote the positions at which the samples can punched out. be 4. Produced from 2B 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 O BSI 08-2000 STDnBSI BS EN 10276-1-ENGL
43、 2000 1624669 0862859 517 Page 10 EN 10276-1 12000 Method A 1. 2. 3. 4. 5. I 2 mI Method B r 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
44、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 O BSI 08-2000 10276-k2000 BSI 389 Chiswick High Road London w4 4ALt BSI - British Standards Institution BSI is the independent nationai body responsible f
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