DIN EN 15605-2010 Copper and copper alloys - Inductively coupled plasma optical emission spectrometry German version EN 15605 2010《铜和铜合金 电感耦合等离子体发射光谱法 德文版本EN 15605-2010》.pdf

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1、December 2010 Translation by DIN-Sprachendienst.English price group 19No 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).I

2、CS 77.120.30!$lX“1735953www.din.deDDIN EN 15605Copper and copper alloys Inductively coupled plasma optical emission spectrometryEnglish translation of DIN EN 15605:2010-12Kupfer und Kupferlegierungen Optische Emissionsspektrometrie mit induktiv gekoppelter PlasmaanregungEnglische bersetzung von DIN

3、EN 15605:2010-12Cuivre et alliages de cuivre Analyse par spectromtrie dmission optique avec source plasma induit par hautefrquenceTraduction anglaise de DIN EN 15605:2010-12SupersedesDIN CEN/TS 15605:2008-02www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be c

4、onsidered authoritative.5111.10 DIN EN 15605:2010-12 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Norm

5、enausschuss Nichteisenmetalle (Nonferrous Metals Standards Committee), Working Committee NA 066-02-06 AA Analysenverfahren fr NE-Metalle. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 IS

6、O 5725-3 DIN ISO 5725-3 Amendments This standard differs from DIN CEN/TS 15605:2008-02 as follows: a) the status of the Technical Specification/prestandard has been changed to that of a full standard; b) precision criteria for methods A and E have been added; c) precision criteria for methods B, C,

7、D and F have been improved and updated; d) method G (specifying the analysis of copper-tin-lead alloys) has been edited on an informative basis (see Annex B), taking into account the poor quality of the precision criteria related to this method. Previous editions DIN CEN/TS 15605: 2008-02 National A

8、nnex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeat

9、ability and reproducibility of a standard measurement method DIN ISO 5725-3, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15605 July 2010 ICS

10、 77.120.30 Supersedes CEN/TS 15605:2007English Version Copper and copper alloys - Inductively coupled plasma optical emission spectrometry Cuivre et alliages de cuivre - Analyse par spectromtrie dmission optique avec source plasma induit par haute frquence Kupfer und Kupferlegierungen - Optische Emi

11、ssionsspektrometrie mit induktiv gekoppelter Plasmaanregung This European Standard was approved by CEN on 12 June 2010. 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

12、 any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language ma

13、de by translation under the responsibility of a CEN member into its own language and notified to the CEN 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, Fin

14、land, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES

15、KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15605:2010: EEN 15605:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 63 Principle 64 R

16、eagents .65 Apparatus 116 Sampling 117 Procedure 117.1 Method A: Coppers . 117.2 Method B: Copper-zinc alloys . 157.3 Method C: Copper-tin alloys 197.4 Method D: Copper-aluminium alloys 237.5 Method E: Copper-beryllium alloys 277.6 Method F: Copper-nickel alloys 318 Expression of results . 359 Preci

17、sion 359.1 Method A Coppers . 359.2 Method B Copper-zinc alloys 369.3 Method C Copper-tin alloys 379.4 Method D Copper-aluminium alloys . 389.5 Method E Copper-beryllium alloys . 399.6 Method F Copper-nickel alloys . 4010 Test report . 40Annex A (informative) Optical emission spectrometer (OES) Sugg

18、ested performance criteria to be checked 41Annex B (informative) Inductively coupled plasma emission spectrometry method for the analysis of Copper-tin-lead alloys 43Bibliography . 49DIN EN 15605:2010-12 EN 15605:2010 (E) 3 Foreword This document (EN 15605:2010) has been prepared by Technical Commit

19、tee CEN/TC 133 “Copper and copper 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 January 2011, and conflicting national standards shall be withdr

20、awn at the latest by January 2011. 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 CEN/TS 15605:2007. Within

21、its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of Analysis“ to revise the following Technical Specification: CEN/TS 15605, Copper and copper alloys Inductively coupled plasma optical emission spectrometry In comparison with the first edition of CEN/TS 15605

22、:2007, the following significant technical changes were made: Revision from a Technical Specification to a European Standard; Method G (specifying the analysis of Copper-tin-lead alloys) is edited under an informative basis (see An-nex B), taking into account the mediocrity of the precision criteria

23、 related to this method; Precision criteria for methods A and E were added; Precision criteria for methods B, C, D and F were improved and up-dated. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European

24、 Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and Unite

25、d Kingdom. DIN EN 15605:2010-12 EN 15605:2010 (E) 4 1 Scope This European Standard specifies six inductively coupled plasma emission spectrometry methods (A to F) for the determination of alloying elements and impurities in copper and copper alloys in the form of unwrought, wrought and cast products

26、. A complementary method, for the analysis of Copper-tin-lead alloys, is described in Annex B (informative). The precision criteria concerning this method do not reach the suitable level, for all the elements specified (zinc and phosphorus, namely). These methods are applicable to the elements liste

27、d in Tables 1 to 6 within the composition ranges shown: Table 1 Coppers Element Mass fraction % min. max. Sn 0,02 0,60Pb 0,02 0,60Zn 0,02 0,60 Fe 0,01 0,60Ni 0,01 0,60Mn 0,01 0,60 Al 0,02 0,60P 0,01 0,40Be 0,01 0,60 Co 0,01 0,60Cd 0,01 0,60Table 2 Copper-zinc alloys Element Mass fraction % min. max.

28、 Sn 0,05 2,00 Pb 0,03 4,00 Zn 10,00 42,00 Fe 0,01 5,00 Ni 0,02 4,00 Mn 0,01 6,00 P 0,01 0,40 Al 0,02 9,00 As 0,01 0,20 DIN EN 15605:2010-12 EN 15605:2010 (E) 5 Table 3 Copper-tin alloys Element Mass fraction % min. max. Sn 3,00 16,00Pb 0,01 9,00 Zn 0,03 6,00 Fe 0,01 1,00 Ni 0,05 7,00 Mn 0,01 0,40 P

29、0,01 0,60 Al 0,01 0,50 Sb 0,02 1,60 As 0,02 0,25 Table 4 Copper-aluminium alloys Element Mass fraction % min. max. Sn 0,02 0,50Pb 0,03 0,50Zn 0,03 1,00 Fe 0,05 7,00 Ni 0,10 8,00 Mn 0,01 5,00 Al 6,00 14,00Cd 0,01 0,50 Mg 0,002 0,15 Table 5 Copper-beryllium alloys Element Mass fraction % min. max. Sn

30、0,02 0,20Pb 0,01 0,20 Zn 0,03 0,20Fe 0,03 0,30 Ni 0,04 2,50Mn 0,006 0,15 Al 0,03 0,20Be 0,08 4,00 Co 0,03 4,00DIN EN 15605:2010-12 EN 15605:2010 (E) 6 Table 6 Copper-nickel alloys Element Mass fraction % min. max. Sn 0,10 0,50 Pb 0,03 0,50 Zn 0,04 2,00 Fe 0,10 4,00 Ni 7,00 35,00Mn 0,02 3,00 Al 0,02

31、0,50 NOTE 1 The ranges specified for each method can be extended or adapted, for the determination of lower mass frac-tions. NOTE 2 Other elements may be included. However such elements and their mass fractions should be carefully checked, taking into account interference, sensitivity, resolution an

32、d linearity criteria for each instrument and each wave-length. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated refer-ences, only the edition cited applies. For undated references, the latest edition of the referenced documen

33、t (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 wrough

34、t products and castings 3 Principle Dissolution of a test portion with hydrochloric and nitric acids. After suitable dilution and addition of an internal reference element, nebulization of the solution into an inductively coupled plasma emission spectrometer and measurement of the intensity of the e

35、mitted light, including that of the internal reference element. 4 Reagents During the analysis, use only reagents of recognised analytical grade and only distilled water or water of equivalent purity. The same reagents should be used for the preparation of calibration solutions and of sample solutio

36、ns. 4.1 Hydrochloric acid, HCl ( = 1,19 g/ml) DIN EN 15605:2010-12 EN 15605:2010 (E) 7 4.2 Hydrochloric acid, solution 1 + 1 Add 500 ml of hydrochloric acid (4.1) to 500 ml of water. 4.3 Nitric acid, HNO3( = 1,40 g/ml) 4.4 Nitric acid, solution 1 + 1 Add 500 ml of nitric acid (4.3) to 500 ml of wate

37、r. 4.5 Hydrofluoric acid, HF (= 1,13 g/ml) 4.6 Sulphuric acid, H2SO4(4,5 mol/l) 4.7 Electrolytic copper 4.8 Zinc granules of 99,999 % purity 4.9 Aluminium stock solution, 10 g/l Al Weigh (5 0,001) g of aluminium (Al 99,99 %) and transfer into a 600 ml beaker. Add 250 ml of hydrochloric acid solution

38、 (4.2) and cover with a watch glass. After cooling to room temperature, transfer the solution quan-titatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 10 mg of Al. 4.10 Aluminium stock solution, 1 g/l Al Weigh (1 0,001) g of

39、aluminium (Al 99,99 %) and transfer into a 400 ml beaker. Add 50 ml of hydrochloric acid solution (4.2) and cover with a watch glass. After cooling to room temperature, transfer the solution quan-titatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml o

40、f this solution contains 1 mg of Al. 4.11 Antimony stock solution, 1 g/l Sb Weigh (0,5 0,001) g of antimony (Sb 99,99 %) and transfer into a 250 ml beaker. Add 50 ml of hydrochlo-ric acid (4.1) and 25 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is disso

41、lved. After cooling to room temperature, transfer the solution quantitatively into a 500 ml one-mark volu-metric flask, containing 100 ml of hydrochloric acid (4.1), dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Sb. 4.12 Arsenic stock solution, 1 g/l As Weigh (0,

42、5 0,001) g of arsenic (As 99,99 %) and transfer into a 250 ml beaker. Add 20 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is dissolved. After cooling to room temperature, transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilut

43、e to the mark with water and mix well. 1 ml of this solution contains 1 mg of As. DIN EN 15605:2010-12 EN 15605:2010 (E) 8 4.13 Beryllium stock solution, 5 g/l Be Weigh (1 0,001) g of beryllium (Be 99,99 %) and transfer into a 250 ml beaker. Add 40 ml of hydrochloric acid (4.1) and cover with a watc

44、h glass. Heat gently until the metal is dissolved. After cooling to room temperature, transfer the solution quantitatively into a 200 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Be. 4.14 Beryllium stock solution, 1 g/l Be Weigh (0,

45、5 0,001) g of beryllium (Be 99,99 %) and transfer into a 250 ml beaker. Add 20 ml of hydrochloric acid (4.1) and cover with a watch glass. Heat gently until the metal is dissolved. After cooling to room tem-perature, transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilut

46、e to the mark with water and mix well. 1 ml of this solution contains 1 mg of Be. 4.15 Cadmium stock solution, 1 g/l Cd Weigh (1 0,001) g of cadmium (Cd 99,99 %) and transfer into a 400 ml beaker. Add 10 ml of nitric acid (4.3) and cover with a watch glass. Heat gently until the metal is dissolved,

47、then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Cd. 4.16 Cobalt stock solution, 5 g/l Co Weigh (1 0,

48、001) g of cobalt (Co 99,99 %) and transfer into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of nitric acid (4.3) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer t

49、he solution quantita-tively into a 200 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Co. 4.17 Cobalt stock solution, 1 g/l Co Weigh (0,5 0,001) g of cobalt (Co 99,99 %) and transfer into a 250 ml beaker. Add 5 ml of hydrochloric acid (4.1) and 5 ml of nitric acid (4.3) and cov

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