1、July 2015Translation by DIN-Sprachendienst.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 77
2、.040.30; 77.120.30!%D90“2332213www.din.deDDIN EN 15079Copper and copper alloys Analysis by spark optical emission spectrometry (S-OES);English version EN 15079:2015,English translation of DIN EN 15079:2015-07Kupfer und Kupferlegierungen Analyse durch optische Emissionsspektrometrie mit Funkenanregun
3、g (F-OES);Englische Fassung EN 15079:2015,Englische bersetzung von DIN EN 15079:2015-07Cuivre et alliages de cuivre Analyse par spectromtrie dmission optique tincelles (SEO-E);Version anglaise EN 15079:2015,Traduction anglaise de DIN EN 15079:2015-07SupersedesDIN EN 15079:2007-08www.beuth.deIn case
4、of doubt, the German-language original shall be considered authoritative.Document comprises 22 pages06.15 DIN EN 15079:2015-07 2 A comma is used as the decimal marker. National foreword This document (EN 15079:2015) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys” (Secr
5、etariat: DIN, Germany). The responsible German body involved in its preparation was the DIN-Normenausschuss Nichteisenmetalle (DIN Standards Committee Nonferrous Metals), Working Committee NA 066-02-06 AA Analysenverfahren fr NE-Metalle. Amendments This standard differs from DIN EN 15079:2007-08 as
6、follows: a) the definitions of terms 3.1 to 3.5 have been rendered more precise; b) in Subclause 7.2.2, the calibration has been improved. Previous editions DIN EN 15079: 2007-08 EN 15079May 2015 ICS 77.040.30; 77.120.30 Supersedes EN 15079:2007English Version Copper and copper alloys - Analysis by
7、spark optical emission spectrometry (S-OES) Cuivre et alliages de cuivre - Analyse par spectromtrie dmission optique tincelles (SEO-E) Kupfer und Kupferlegierungen - Analyse durch optische Emissionsspektrometrie mit Funkenanregung (F-OES) This European Standard was approved by CEN on 24 April 2015.
8、CEN members are bound to comply with the CEN/CENELEC 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 such national standards may be obtained on a
9、pplication to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three 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 the CEN-CENELEC
10、 Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
11、Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved
12、worldwide for CEN national Members. Ref. No. EN 15079:2015 EEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGEN 15079:2015 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Terms and def
13、initions .4 4 Principle 5 5 Apparatus .5 5.1 Optical emission spectrometer 5 5.2 Apparatus for sample surface preparation .5 6 Sampling .5 7 Procedure .6 7.1 Surface preparation .6 7.2 Calibration procedures .6 7.2.1 General 6 7.2.2 Calibration 7 7.2.3 Recalibration 7 7.2.4 Type recalibration 7 7.3
14、Analysis 7 7.3.1 Preparation of analytical programs .7 7.3.2 Analysis method 8 7.3.3 Number of sparks on test samples 8 7.3.4 Status check of the apparatus 8 8 Expression of results 8 9 Precision .9 10 Test report 9 Annex A (informative) Wavelengths for spectrometric analysis and typical calibration
15、 ranges for copper and copper alloys 10 Annex B (informative) Wavelengths, background equivalent concentrations (BEC) and detection limits (DL) for pure copper . 17 Bibliography . 20 DIN EN 15079:2015-07EN 15079:2015 (E) 3 Foreword This document (EN 15079:2015) has been prepared by Technical Committ
16、ee CEN/TC 133 “Copper and cop-per alloys”, the secretariat of which is held by DIN. 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 2015, and conflicting national standards shall be withd
17、rawn at the latest by November 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 15079:2007. Within it
18、s programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to revise this standard: EN 15079:2007, Copper and copper alloys Analysis by spark source optical emission spectrometry (S-OES). In comparison with EN 15079:2007, the following changes were made: a)
19、Definitions 3.1 to 3.5 have been improved; b) 7.2.2 Calibration has been modified. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Repu
20、blic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN
21、EN 15079:2015-07EN 15079:2015 (E) 4 1 Scope This European Standard specifies a routine method for the analysis of copper and copper alloys by spark optical emission spectrometry (S-OES). The method is applicable to all elements except copper commonly present in copper and copper alloys as impurities
22、 or minor or main constituents, which can be determined by S-OES. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references,
23、the latest edition of the referenced document (including any amendments) applies. ISO 1811-1, Copper and copper alloys Selection and preparation of samples for chemical analysis Part 1: Sampling of cast unwrought products ISO 1811-2, Copper and copper alloys Selection and preparation of samples for
24、chemical analysis Part 2: Sampling of wrought products and castings 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 reference material RM material, sufficiently homogeneous and stable with respect to one or more specified properties which has
25、 been established to be fit for its intended use in a measurement process SOURCE: ISO GUIDE 30:1992/Amd.1:2008, definition 2.1 3.2 certified reference material CRM reference material characterized by a metrologically valid procedure for one or more specified properties, ac-companied by a certificate
26、, that provides the value of the specified property, its associated uncertainty, and a statement of metrological traceability SOURCE: ISO GUIDE 30:1992/Amd.1:2008, definition 2.2 3.3 test sample representative quantity of material for testing purposes 3.4 drift control samples series of homogeneous
27、materials that contain all the elements which have been calibrated and that cover the low, mid and high points of the calibration range for each element, used to detect variations over time in these points Note 1 to entry: Drift control samples can also be used for statistical process control (SPC)
28、of the instrument. DIN EN 15079:2015-07EN 15079:2015 (E) 5 3.5 recalibration samples samples at both low and high points of the calibration ranges used to recalibrate the spectrometer Note 1 to entry: These samples are measured during the calibration procedure and the intensities obtained are stored
29、 in the computer according to the manufacturers instructions. Note 2 to entry: No chemical analyses are necessary, but the homogeneity of these samples should be carefully eval-uated. 3.6 quality control sample sample with known composition which is analysed in the same way as the test sample to che
30、ck the trueness of the analytical results 4 Principle Measurement of the intensity of the radiation, whose wavelength is characteristic of each element, generated by a spark resulting from the application of an electrical discharge between the sample, as one electrode, and an inert counter-electrode
31、. Concentrations of elements are determined by relating the measured intensities of test samples to calibration curves prepared from reference materials. 5 Apparatus 5.1 Optical emission spectrometer Spectrometer with spark source capable of measuring the intensities of the optical radiation emitted
32、 at specific wavelengths by the elements present in the material. The wavelengths generally used are given in Annex A. 5.2 Apparatus for sample surface preparation The most common surface preparation techniques for copper and copper alloys are turning and milling or grinding for copper, provided tha
33、t the composition of the surface shall not be influenced. The lathe, milling machine or any other machines used for surface preparation shall be able to produce a surface that conforms to the requirements of 7.1. WARNING The appropriate safety recommendations for the use of mechanical apparatus shal
34、l be observed. These operations shall be carried out only by properly trained personnel wearing appropriate personal protective equipment. 6 Sampling Sampling shall be carried out in accordance with ISO 1811-1 or ISO 1811-2, as appropriate. The sample needs to be sufficiently homogeneous with regard
35、 to the spark impact. The measuring surface should be free of defects. DIN EN 15079:2015-07EN 15079:2015 (E) 6 7 Procedure 7.1 Surface preparation 7.1.1 The surface of the sample shall be prepared to a finish that is sufficiently flat and smooth in order to tighten the sample chamber, and shall be r
36、easonably free from contaminants, pores, cracks, inclusions and shrinkage cavities which might otherwise affect analytical results. In order to avoid variation of results due to the influence of surface finish, the same method of preparation shall be used for all samples. To avoid cross-contaminatio
37、n between different sample materials, for example pure copper and copper alloys, all relevant components of the machine shall be thoroughly cleaned before use or separate tools shall be used. Once the surface has been prepared, avoid any contamination, for example fingerprints. Measurements shall be
38、 carried out soon after surface preparation. Samples should be stored, until the time of later measurement, in a desiccator. 7.1.2 The turning, milling or grinding shall be carried out at a suitable speed to avoid undue heating of the sample surface, which might otherwise lead to bias in analysis. A
39、ny lubricants (e.g. propanol) used shall be selected to ensure that they do not affect the analytical result. 7.2 Calibration procedures 7.2.1 General 7.2.1.1 Calibration process The calibration process is subdivided into calibration and drift compensation by recalibration. 7.2.1.2 Range of calibrat
40、ion The range of calibration for an element shall extend well below the minimum content reported in the list of alloys composition and above the maximum content reported in the same list, taking into account that the lowest limit should be at least three times the detection limit. 7.2.1.3 Number of
41、sparks on calibration samples The number of sparks carried out on each reference material for calibration shall be not less than four. The spark areas shall be distributed over the prepared surface. Centre and border of the sample have to be avoided. All measurements shall be examined; if any measur
42、ement is obviously defective, further sparks shall be carried out to obtain the minimum four acceptable measurements. The average of the four acceptable measurements is used for calibration. The influence of temperature is very important for direct measurement methods. The sample should be cooled to
43、 ambient temperature between each spark. DIN EN 15079:2015-07EN 15079:2015 (E) 7 7.2.2 Calibration The calibration of the spectrometer is carried out by using a series of certified reference materials which have the same or at least similar matrix and metallurgical structure as the samples to be ana
44、lysed, in order to calculate the calibration functions from which the analysis of test samples can be obtained. The content range of the certified reference materials used shall cover that of all the samples to be analysed within each specific analytical program. For each element in each reference m
45、aterial the mean intensity is correlated to the corresponding certified content and a regression is calculated. The calibration functions are usually stored within a computer, connected to the spectrometer. These calibration functions are 1stor 2nddegree mathematical equations. The calibration is no
46、rmally done when the apparatus is installed. The calibration shall be in accordance with the spectrometer manufacturers instruction manual, using the appropriate certified reference materials, if available. If no certified reference materials are available, reference materials with an accurate analy
47、sis shall be used. The trueness of the analytical procedure is checked by measuring a set of certified reference materials or if not available a set of reference materials not used in the calibration. These reference materials shall cover at least the low, mid and high points of the calibration rang
48、e for each element. 7.2.3 Recalibration Drifts of the spectrometer readings shall be corrected using a recalibration procedure as described in the manufacturers instruction manual. Recalibrations can be done either for all analytical channels (global recalibration), or only for individual analytical
49、 channels (selective recalibration). Recalibration can either be done periodically or due to a deviation from statistical process control (SPC) limits (see 7.3.4). When a periodical recalibration procedure is used, the period depends on the stability of the spectrometer and has to be established by a stability check of the spectrometer. The stability check shall be repeated at appropriate intervals. NOTE The same set of check samples can be used both for drift con
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