SIST EN 15079:2015
(Main)Copper and copper alloys - Analysis by spark source optical emission spectrometry (S-OES)
Copper and copper alloys - Analysis by spark source optical emission spectrometry (S-OES)
This European Standard specifies a routine method for the analysis of copper and copper alloys by spark source optical emission spectrometry (S-OES). The method is applicable to all elements except copper commonly present in copper and copper alloys present as impurities or minor or main constituents, and detectable by S-OES.
Kupfer und Kupferlegierungen - Analyse durch optische Emissionsspektrometrie mit Funkenanregung (F-OES)
Diese Europäische Norm legt ein Routineverfahren für die Analyse von Kupfer und Kupferlegierungen mit optischer Emissionsspektrometrie mit Funkenanregung (F OES) fest. Das Verfahren ist anwendbar auf alle Elemente mit Ausnahme von Kupfer, welche als Verunreinigungen oder Neben oder Hauptbestandteile in Kupfer oder Kupferlegierungen vorliegen und die mit F OES bestimmbar sind.
Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique à étincelles (SEO-E)
La présente Norme européenne spécifie une méthode de routine pour l’analyse du cuivre et des alliages de cuivre par spectrométrie d’émission optique à étincelles (SEO-E). Cette méthode s'applique à tous les éléments généralement présents dans le cuivre et les alliages de cuivre, à l'exception du cuivre lui-même, tels que les impuretés ou les constituants mineurs ou principaux, pouvant être déterminés par SEO-E.
Baker in bakrove zlitine - Analiza z optično emisijsko spektrometrijo, inducirano z iskrenjem (S-OES)
Ta evropski standard določa rutinsko metodo za analizo bakra in bakrovih zlitin z optično emisijsko spektrometrijo, inducirano z iskrenjem (S-OES). Ta metoda se uporablja za vse elemente, razen za baker, ki je običajno prisoten v bakru in bakrovih zlitinah, ki so prisotni kot nečistoče ali manj ali bolj pomembne sestavine, pri čemer se jih zazna s S-OES.
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kupfer und Kupferlegierungen - Analyse durch optische Emissionsspektrometrie mit Funkenanregung (F-OES)Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique à étincelles (SEO-E)Copper and copper alloys - Analysis by spark source optical emission spectrometry (S-OES)77.120.30Baker in bakrove zlitineCopper and copper alloys77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 15079:2015SIST EN 15079:2015en,fr,de01-september-2015SIST EN 15079:2015SLOVENSKI
STANDARDSIST EN 15079:20071DGRPHãþD
SIST EN 15079:2015
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15079
May 2015 ICS 77.040.30; 77.120.30 Supersedes EN 15079:2007English Version
Copper and copper alloys - Analysis by spark optical emission spectrometry (S-OES)
Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique à étincelles (SEO-E)
Kupfer und Kupferlegierungen - Analyse durch optische Emissionsspektrometrie mit Funkenanregung (F-OES) This European Standard was approved by CEN on 24 April 2015.
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 application 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 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, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15079:2015 ESIST EN 15079:2015
EN 15079:2015 (E) 2 Contents Page Foreword .3 1 Scope .4 2 Normative references .4 3 Terms and definitions .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 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 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
SIST EN 15079:2015
EN 15079:2015 (E)
3 Foreword This document (EN 15079:2015) has been prepared by Technical Committee 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 withdrawn 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 its 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) 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 Republic, 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. SIST EN 15079:2015
EN 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 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, 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 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 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, 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 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) of the instrument. SIST EN 15079:2015
EN 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 in the computer according to the manufacturer's 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 check 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. 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 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 that 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 shall 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 to the spark impact. The measuring surface should be free of defects. SIST EN 15079:2015
EN 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 reasonably 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-contamination 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 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. Any 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 calibration 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 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 measurement 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 ambient temperature between each spark. SIST EN 15079:2015
EN 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 analysed, 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 ea
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kupfer und Kupferlegierungen - Analyse durch optische Emissionsspektrometrie mit Funkenanregung (F-OES)Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique à étincelles (SEO-E)Copper and copper alloys - Analysis by spark source optical emission spectrometry (S-OES)77.120.30Baker in bakrove zlitineCopper and copper alloys77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:FprEN 15079kSIST FprEN 15079:2015en,fr,de01-januar-2015kSIST FprEN 15079:2015SLOVENSKI
STANDARD
kSIST FprEN 15079:2015
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
FINAL DRAFT
FprEN 15079
October 2014 ICS 77.040.30; 77.120.30 Will supersede EN 15079:2007English Version
Copper and copper alloys - Analysis by spark source optical emission spectrometry (S-OES)
Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique à étincelles (SEO-E)
Kupfer und Kupferlegierungen - Analyse durch optische Emissionsspektrometrie mit Funkenanregung (F-OES) This draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical Committee CEN/TC 133.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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 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, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. FprEN 15079:2014 EkSIST FprEN 15079:2015
FprEN 15079:2014 (E) 2 Contents Page Foreword .3 1 Scope .4 2 Normative references .4 3 Terms and definitions .4 4 Principle .5 5 Apparatus .5 6 Sampling .5 7 Procedure .6 8 Expression of results .8 9 Precision .8 10 Test report .9 Annex A (informative)
Wavelengths for spectrometric analysis and typical calibration ranges for copper and copper alloys . 10 Annex B (informative)
Wavelengths, background equivalent concentrations (BEC) and detection limits (DL) for pure copper . 15 Bibliography . 18
kSIST FprEN 15079:2015
FprEN 15079:2014 (E)
3 Foreword This document (FprEN 15079:2014) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which is held by DIN. This document is currently submitted to the Unique Acceptance Procedure. This document will supersede EN 15079:2007. Within its 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) Definitions 3.1 to 3.5 have been improved; b) 7.2.2 Calibration has been modified. kSIST FprEN 15079:2015
FprEN 15079:2014 (E) 4 1 Scope This European Standard specifies a routine method for the analysis of copper and copper alloys by spark source optical emission spectrometry (S-OES). The method is applicable to all elements except copper commonly present in copper and copper alloys as impurities 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, 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 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 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, 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 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) of the instrument. kSIST FprEN 15079:2015
FprEN 15079:2014 (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 in the computer according to the manufacturer's 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 check 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. 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 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 that 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 shall 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 to the spark impact. The measuring surface should be free of defects. kSIST FprEN 15079:2015
FprEN 15079:2014 (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, reasonably free from contaminants, pores, cracks, inclusions and shrinkage cavi-ties 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-contamination 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 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. Any 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 calibration 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 concentration 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 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 measurement 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 ambient temperature between each spark. 7.2.2 Calibration The calibration of the spectrometer is carried out using a series of certified reference materials similar matrix and metallurgical structure as the samples to be analysed to calculate 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 kSIST FprEN 15079:2015
FprEN 15079:2014 (E)
7 reference material 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 1st or 2nd degree mathematical equations. The calibration is normally done when the apparatus is installed. The calibration shall be in accordance with the spectrometer manufacturer's instruction manual, using the appropriate certified reference materials, if available. If no certified reference materials are available, reference materials with an accurate analysis 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 range for each element. 7.2.3 Recalibration Drifts of the spectrometer readings shall be corrected using a recalibration procedure as described in the manufacturer's instruction manual. Recalibrations can be done either for all analytical channels (global recalibration), or only for individual analytical channels (selecti
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