EN 15063-2-2006 en Copper and copper alloys - Determination of main constituents and impurities by wavelength dispersive X-ray fluorescence spectrometry (XRF) - Part 2 Routine meth.pdf

1、BRITISH STANDARDBS EN 15063-2:2006Copper and copper alloys Determination of main constituents and impurities by wavelength dispersive X-ray fluorescence spectrometry (XRF) Part 2: Routine methodThe European Standard EN 15063-2:2006 has the status of a British StandardICS 77.120.30g49g50g3g38g50g51g6

2、0g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 15063-2:2006This British Standard was published under the authority of the Standards Policy and Strategy Committe

3、e on 30 November 2006 BSI 2006ISBN 0 580 49685 6National forewordThis British Standard was published by BSI. It is the UK implementation of EN 15063-2:2006.The UK participation in its preparation was entrusted to Technical Committee NFE/34, Copper and copper alloys.A list of organizations represente

4、d on NFE/34 can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments issued since

5、publicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15063-2November 2006ICS 77.120.30English VersionCopper and copper alloys - Determination of main constituentsand impurities by wavelength dispersive X-ray fluorescencespectrometry (XRF) - Part 2: Routine methodCuivre

6、et alliages de cuivre - Dtermination des lmentsprincipaux et des impurets par analyse spectromtriquede fluorescence X dispersion en longueur donde (XRF) -Partie 2 : Mthode de routineKupfer und Kupferlegierungen - Bestimmung vonHauptbestandteilen und Verunreinigungen durchwellenlngendispersive Rntgen

7、fluoreszenzanalyse (RFA) -Teil 2: RoutineverfahrenThis European Standard was approved by CEN on 22 September 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any al

8、teration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by trans

9、lationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hunga

10、ry, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue

11、 de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15063-2:2006: EEN 15063-2:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Terms and definitions .4 5 Apparatus

12、 .4 6 Sampling.6 7 Procedure .6 8 Expression of results 8 9 Precision.8 10 Test report 8 Annex A (informative) Conditions for the analysis9 Bibliography 10 EN 15063-2:2006 (E) 3 Foreword This document (EN 15063-2:2006) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, t

13、he 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 May 2007, and conflicting national standards shall be withdrawn at the latest by May 2007. Within its progra

14、mme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the following standard: EN 15063-2, Copper and copper alloys Determination of main constituents and impurities by wavelength dispersive X-ray fluorescence spectrometry (XRF) Part 2: Routine method

15、 This is one of two parts of the standard for the determination of main constituents and impurities in copper and copper alloys. The other part is: EN 15063-1, Copper and copper alloys Determination of main constituents and impurities by wavelength dispersive X-ray fluorescence spectrometry (XRF) Pa

16、rt 1: Guidelines to the routine method According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Den-mark, Estonia, Finland, France, Germany, Greece, Hung

17、ary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxem-bourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzer-land and United Kingdom. EN 15063-2:2006 (E) 4 1 Scope This part of this European Standard specifies a routine method for analysing copper a

18、nd copper alloys by wavelength dispersive X-ray fluorescence spectrometry. The method is applicable to: all elements detectable by XRF: impurities, minor and main constituents; analysis of either unwrought, including chill-cast or wrought products. 2 Normative references The following referenced doc

19、uments are indispensable for the application of this European Standard. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 15063-1:2006, Copper and copper alloys Determination of main cons

20、tituents and impurities by wave-length dispersive X-ray fluorescence spectrometry (XRF) Part 1: Guidelines to the routine method 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 a

21、lloys Selection and preparation of samples for chemical analysis Part 2: Sampling of wrought products and castings 3 Principle An appropriately cleaned test specimen is irradiated by an X-ray-beam of high energy. The secondary X-rays produced are dispersed by means of crystals and the intensities ar

22、e measured by detectors, usually counters at selected characteristics wavelengths. Concentration of the elements is determined by relating the measured intensities from the sample under test to analytical curves prepared from certified reference materials (CRMs) or reference materials (RMs). Fixed c

23、hannels or a sequential system are used to provide simultaneous or sequential determinations of element concentrations. 4 Terms and definitions For the purposes of this European Standard, the terms and definitions given in EN 15063-1:2006 apply. 5 Apparatus 5.1 Sample preparation equipment Suitable

24、machine; lathe, milling or grinding machine. NOTE Surface contamination should be avoided. EN 15063-2:2006 (E) 5 5.2 X-ray fluorescence spectrometer Simultaneous or sequential wavelength dispersive spectrometer. NOTE This test method is written for use with commercially-available instruments. 5.3 X-

25、ray tube Tube with an anode made of a high-purity element. NOTE 1 Rhodium is recommended as the material of the anode for analysis of copper and copper alloys. NOTE 2 Considering a list of elements to be analysed in a copper matrix, it is advisable to check the tube power supply in order to set the

26、right voltage in accordance with the manufacturers instructions. The Voltage shall be adjusted to produce secondary fluorescence, according to the following equation: Uf= 12396/abs(1) where Ufis the minimum voltage required for exciting the line of interest; absis the wavelength of the absorption ed

27、ge of the fluorescent element. If a K line is used, the K absorption edge is used. If an L line is used, the L absorption edge is used. Ideally, the operating voltage should approximate to or exceed 3 Uf. 5.4 Analysing crystal To cover all elements specified in this method, flat or curved crystals,

28、made of LiF and PET (for elements with a low atomic number), are required. Crystals of other materials, optimized for individual elements, can also be used (see Table A.1). 5.5 Collimators For sequential instruments, a two collimator system is necessary. A coarse collimator for elements with a low a

29、tomic number (atomic no. approx. 22) and a fine collimator for elements with a high atomic number. 5.6 Detectors One scintillation counter (SC) for elements with a high atomic number and one gas-flow (FC) proportional elements with a low atomic number. Sealed proportional counters can also be used.

30、NOTE In case of use of gas flow detectors, P 10 gas (90 % argon mixed with 10 % methane) is needed. 5.7 Vacuum System A vacuum system capable to keep the pressure at constant level of 13 Pa or less. EN 15063-2:2006 (E) 6 5.8 Data collection system An electronic circuit capable of amplifying and inte

31、grating pulses received from the counters and a computer-system with a sufficient software package capable of calculating concentrations based on the measured in-tensities. 6 Sampling Sampling shall be carried out in accordance with ISO 1811-1 or ISO 1811-2 as appropriate. 7 Procedure 7.1 Surface pr

32、eparation 7.1.1 A face of the sample shall be prepared by an appropriate method, e.g. turning, milling or grinding so that it is sufficiently flat and smooth, reasonably free from contaminants, pores, cracks, inclusions and shrink-age cavities. In order to avoid variation in results due to the influ

33、ence of the surface, the same method of preparation shall be used for all samples (test samples and reference material). To avoid cross-contamination between different materials, for example pure copper and copper alloys, all relevant components of the machine shall be thoroughly cleaned before use.

34、 Once the surface has been prepared, it shall be kept clean to avoid any contamination, for example finger-prints. If necessary clean the surface, for example with pure ethanol, before measuring. NOTE Measurements should be carried out as soon as possible after any surface preparation. Samples shoul

35、d be stored in a desiccator until the time of measurement. 7.1.2 Turning, milling or grinding shall be carried out at a suitable rate to avoid undue heating of the sample, which might otherwise cause changes in the sample and lead to variations in analysis. Any lubricants (e.g. propanol) used shall

36、be selected to ensure that they do not affect the analytical result. 7.2 Preparation of apparatus Prepare the instrument for operation according to the manufacturers instructions. Since most of the instru-ments are used for routine analysis it is assumed that they are operating, and in most cases, a

37、re already cali-brated for copper and copper alloys. Verify the calibration status using CRMs or, if not available, RMs. If the instrument has been turned off for a long period (several hours), ensure that the conditions have stabi-lized before starting measuring, e.g. temperature and vacuum. Safety

38、 precautions and national regulations for X-ray equipment shall be observed. NOTE X-ray equipment should be used only under the guidance and supervision of a responsible, qualified person. EN 15063-2:2006 (E) 7 7.3 Measurements Load and measure the samples in accordance with the manufacturers instru

39、ction manual. Ensure that the sample is correctly fixed in the sample cup. Different grain size dimensions of the samples analysed, compared with the calibration standards or different surface finishes, due to tool wear during preparation of the samples may cause different elemental responses, by wh

40、ich the total percentage of the elements analysed varies from 100 %. If that is the case, each element may be fully re-proportioned using suitable software. To avoid machining striations influencing measurements, it is usual for instruments to be equipped with a sample spinner. If that is not the ca

41、se, the sample should be orientated so that the relation between the X-ray beam and the striations is always the same from measurement to measurement. 7.4 Calibration The instrument shall be calibrated upon installation, after major repairs, or as indicated by SPC-data. To com-pensate for the instru

42、ments day to day drift, recalibration procedures shall be followed. If a new calibration is performed, follow the calibration strategy according to the guideline, see EN 15063-1. Typical operating conditions for analysing copper and copper alloys are given in Table A.1 of Annex A of this standard. U

43、sing the same sample preparation, measure the calibration samples together with the recalibration samples according to the manufacturers instruction manual. Make regression calculations and store the coefficients. Verify the calibration by measuring a set of CRMs or, if not available, RMs not used i

44、n the calibration and that cover at least the low, mid and high points of the calibration range for each element. Matrix effects might exist between the various elements in the sample. To compensate for inter-element ef-fects, mathematical corrections shall be applied. A variety of computer programm

45、es for correction are com-monly used and included in the software package from the manufactures. 7.5 Recalibration To correct for day to day variations, a recalibration (reference measurement) procedure shall be used. Recali-bration actions shall be based on the result of checking the instruments pe

46、rformance (sample preparation eliminated) using drift control samples. The instruments performance shall be checked at least every 6 h to 8 h or before and after the measuring a set of test samples. After recalibration, a set of Drift Control Samples or RMs not used in the recalibration procedure sh

47、all be measured. If the calibration is still outside the control limits, check the whole measurement system carefully (x-ray-tube, detectors, ) and after a new standardization (reference measurement), a recalibration or calibration proce-dure shall be undertaken. 7.6 Control of the instrument status

48、 Any change from the original instrument status (e.g. drifts) shall be checked at regular intervals by analysing samples for drift control or reference materials in accordance with the spectrometer manufacturers instruction manual. It is common practice to document the status of the instrument using

49、 control charts. The difference between the results of these control measurements and their reference values are plotted continually on a control chart. If the values fall outside the control limits, then further actions (e.g. recalibration, further control measurements, new calibration) shall be taken. EN 15063-2:2006 (E) 8 The period between checking the instruments status depends on the stability of the instrument and analytical assignment and can be derived from the control charts. In addition, a control measurement shall always be