DIN ISO 16592-2015 Microbeam analysis - Electron probe microanalysis - Guidelines for determining the carbon content of steels using a calibration curve method (ISO 16592 2012)《微光束.pdf
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1、December 2015 English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 71.040.50!%JwX“2398453www.din.d
2、eDIN ISO 16592Microbeam analysis Electron probe microanalysis Guidelines for determining the carbon content of steels using a English translation of DIN ISO 16592:2015-12Mikrobereichsanalyse Elektronenstrahl-Mikroanalyse Leitfaden fr die Bestimmung des Kohlenstoffgehalts von Sthlen mittels einer Kal
3、ibrierkurven-Methode (ISO 16592:2012),Englische bersetzung von DIN ISO 16592:2015-12Analyse par microfaisceaux Analyse par microsonde lectronique (microsonde de Castaing) Lignes directrices pour le dosage du carbone dans les aciers par la droite dtalonnage (ISO 16592:2012),Traduction anglaise de DIN
4、 ISO 16592:2015-12www.beuth.deDocument comprises 15 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.calibration curve method (ISO 16592:2012),12.15National Annex NA (informative) Bibliography 3 1 Scope 4 2 Procedure .4 2.1 Gene
5、ral 4 2.2 Reference materials .4 2.3 Specimen preparation .4 2.4 Measurement of carbon K X-ray intensity 5 2.5 Background subtraction .6 2.6 Establishment of the calibration curve .7 3 Evaluation of uncertainty 9 4 Test report 9 Annex A (informative) Method of estimating the uncertainty of the calcu
6、lated value using a calibration curve 11 Annex B (informative) A practical example of the determination of the mass fraction of carbon and the evaluation of uncertainty in a steel 13 Bibliography 15 A comma is used as the decimal marker. Contents Page National foreword 3DIN ISO 16592:2015-12 2 Natio
7、nal foreword This document (ISO 16592:2012) has been prepared by Technical Committee ISO/TC 202 “Microbeam analysis” (Secretariat: SAC, China). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committe
8、e NA 062-08-18 AA Elektronenmikroskopie und Mikrobereichsanalyse. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. DIN and/or DKE shall not be held responsible for identifying any or all such patent rights. The DIN Standards corres
9、ponding to the International Standards referred to in this document are as follows: ISO 5725-6 DIN ISO 5725-6 ISO/IEC 17025 DIN EN ISO/IEC 17025 ISO 22309 DIN EN ISO 22309 National Annex NA (informative) Bibliography DIN EN ISO/IEC 17025, General requirements for the competence of testing and calibr
10、ation laboratories DIN ISO 5725-6, Accuracy (trueness and precision) of measurement methods and results Part 6: Use in practice of accuracy values DIN ISO 22309, Microbeam analysis Quantitative analysis using energy-dispersive spectrometry (EDS) for elements with an atomic number of 11 (Na) or above
11、 DIN ISO 16592:2015-12 3Microbeam analysis Electron probe microanalysis Guidelines for determining the carbon content of steels using a calibration curve method1 ScopeThis International Standard gives guidance on a method for the determination of the carbon content in steels containing other alloyin
12、g elements (less than 1 % to 2 % by mass) using the calibration curve method. It specifies the sample preparation, X-ray detection, establishment of the calibration curve and the procedure for the determination of the uncertainty of the measured carbon content. It is applicable to steels containing
13、a mass fraction of carbon of less than 1,0 %. The method is not applicable to steels with higher carbon contents, which could significantly affect the accuracy of the analysis results.This International Standard applies to analyses performed using normal beam incidence and wavelength-dispersive X-ra
14、y spectrometry; it is not designed to be used for energy-dispersive X-ray spectrometry.2 Procedure2.1 GeneralIn order to determine the carbon content in steels using a calibration curve, suitable reference materials should be prepared. For accurate analysis, extreme care should be used to prevent ca
15、rbon contamination which would otherwise increase the apparent carbon content of the specimen.The measurement of C K intensity should be carried out using the same procedures for the specimen and the reference materials; that is, specimen preparation, beam energy, beam current, beam diameter, point
16、counting mode, step between points in case of line analysis, and also the method of background subtraction.2.2 Reference materialsTo establish the calibration curve to determine the carbon content, a suitable reference material or set of reference materials should be used. Examples of reference mate
17、rials are as follows: Fe-C solid-solution reference materials which are manufactured by quenching from the austenite region at high temperature; these reference materials should be homogeneous and contain different carbon concentrations; Fe-C compound Fe3C1.Reference materials with a different C K p
18、eak shape compared to the unknown materials should not be used because the use of these reference materials causes a lowering of the quantitative accuracy.2.3 Specimen preparation2.3.1 GeneralThe presence of carbon and/or its compounds as contamination on the specimen surface as a result of specimen
19、 preparation significantly affects the accuracy of carbon analysis. Extreme care should be used to prevent this contamination. The specimen preparation (mounting, grinding and polishing) procedures should be the same for both the reference material and the unknown material.DIN ISO 16592:2015-12 4 2.
20、3.2 Specimen mountingAlthough it is often possible to analyse a specimen without the use of a mounting medium, for small or irregularly shaped specimens mounting will be necessary. It is important to realize that the mounting material can act as a source of carbon contamination. Various mounting med
21、ia are available, such as Bakelite and copper-filled or aluminium-filled (or even graphite-filled) resins, and it is recommended that the user evaluate the different types.Where a mounting medium is used, areas chosen for analysis should, if possible, be close to the centre of the specimen to avoid
22、smearing effects close to the mounting medium/specimen interface.A conductive path must be established from the specimen or reference material to ground to prevent charging.Outgassing of the specimen-mounting medium should be minimized. Virtual leaks from porosity in the specimen and gaps in the mou
23、nting medium/specimen interface will degrade the vacuum, resulting in higher contamination levels.2.3.3 Specimen polishing and cleaningThe surface finish of the specimen to be examined should be flat, clean and dry. The specimen should be prepared in the standard metallographic manner, using silicon
24、 carbide papers for grinding and diamond-impregnated pads for polishing, etc. Final polishing should be with a carbon-free material such as alumina powder. After polishing, it is important to thoroughly clean the specimen so as to remove any residue resulting from the preparation, using a carbon-fre
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