DIN EN 16117-2-2013 Copper and copper alloys Determination of copper content Part 2 Electrolytic determination of copper in materials with copper content higher than 99 80 % German.pdf

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1、February 2013 Translation by DIN-Sprachendienst.English price group 9No 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).IC

2、S 77.120.30!$Fz“1943587www.din.deDDIN EN 16117-2Copper and copper alloys Determination of copper content Part 2: Electrolytic determination of copper in materials with coppercontent higher than 99,80 %;English version EN 16117-2:2012,English translation of DIN EN 16117-2:2013-02Kupfer und Kupferlegi

3、erungen Bestimmung des Kupfergehaltes Teil 2: Elektrolytische Bestimmung von Kupfer in Werkstoffen mit einem Kupfergehaltgrer als 99,80 %;Englische Fassung EN 16117-2:2012,Englische bersetzung von DIN EN 16117-2:2013-02Cuivre et alliages de cuivre Dtermination de la teneur en cuivre Partie 2: Dtermi

4、nation par lectrogravimtrie du cuivre dans les matriaux ayant uneteneur en cuivre suprieure 99,80 %;Version anglaise EN 16117-2:2012,Traduction anglaise de DIN EN 16117-2:2013-02SupersedesDIN 50502:1998-05www.beuth.deDocument comprises 13 pagesIn case of doubt, the German-language original shall be

5、considered authoritative.01.13DIN EN 16117-2:2013-02 2 A comma is used as the decimal marker. National foreword This document (EN 16117-2:2012) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys” (Secretariat: DIN, Germany). The responsible German body involved in its prep

6、aration was the Normenausschuss 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

7、-2 DIN ISO 5725-2 ISO 5725-3 DIN ISO 5725-3 Amendments This standard differs from DIN 50502:1998-05 as follows: a) the standard has been converted into a European Standard; b) when calculating the copper content, the mass of residual copper found in the spent electrolyte is taken into account (see E

8、quation (1) and new Annex A); c) Clause 9 “Precision” has been completely revised. Previous editions DIN 50502: 1973-10, 1992-08, 1998-05 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and d

9、efinitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 5725-3, Accuracy (trueness and precision) of measurement methods and results Part 3

10、: Intermediate measures of the precision of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16117-2 November 2012 ICS 77.120.30 English Version Copper and copper alloys - Determination of copper content - Part 2: Electrolytic determination of copper in materials wi

11、th copper content higher than 99,80 % Cuivre et alliages de cuivre - Dtermination de la teneur en cuivre - Partie 2 : Dtermination par lectrogravimtrie du cuivre dans les matriaux ayant une teneur en cuivre suprieure 99,80 % Kupfer und Kupferlegierungen - Bestimmung des Kupfergehaltes - Teil 2: Elek

12、trolytische Bestimmung von Kupfer in Werkstoffen mit einem Kupfergehalt grer als 99,80 % This European Standard was approved by CEN on 20 October 2012. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the statu

13、s 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, Ger

14、man). 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, Croati

15、a, 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 Uni

16、ted Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16117-2:201

17、2: EEN 16117-2:2012 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Sampling .57 Procedure .58 Expression of results 69 Precision .610 Test report 7Annex A (normative) Spent electrolyte Determination of residual copper Flame atomic absorption

18、spectrometric method (FAAS) 8Bibliography . 11DIN EN 16117-2:2013-02 EN 16117-2:2012 (E) 3 Foreword This document (EN 16117-2:2012) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which is held by DIN. This European Standard shall be given the statu

19、s of a national standard, either by publication of an identical text or by endorsement, at the latest by May 2013, and conflicting national standards shall be withdrawn at the latest by May 2013. Attention is drawn to the possibility that some of the elements of this document may be the subject of p

20、atent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the following standard: EN 16117-2, Copper and copper alloys Determin

21、ation of copper content Part 2: Electrolytic determination of copper in materials with copper content higher than 99,80 %. This is one of two parts of the standard for the determination of the copper content of copper and copper alloys. The other part is: EN 16117-1, Copper and copper alloys Determi

22、nation of copper content Part 1: Electrolytic determination of copper in materials with copper content less than 99,85 %. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium

23、, 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, Switzerla

24、nd, Turkey and the United Kingdom. DIN EN 16117-2:2013-02 EN 16117-2:2012 (E) 4 1 Scope This European Standard specifies an electrolytic method for the determination of the copper content of unalloyed copper materials with a copper content higher than 99,80 % (mass fraction) in the form of castings,

25、 wrought and unwrought products. Silver, if present, is co-deposited and is reported as copper. Approximately one-half of any selenium and tellurium present will co-deposit. Bismuth, if present, also interferes. 2 Normative references The following documents, in whole or in part, are normatively ref

26、erenced 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 sample

27、s 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 Principle Dissolution of a test portion in a nitric and sulphuric acid mixture. El

28、ectrolytic deposition of the copper on a platinum cathode of known weight with subsequent weighing of the cathode together with the electrodeposited copper. Determination of residual copper in the spent electrolyte by atomic absorption spectrometry. 4 Reagents During the analysis use only reagents o

29、f recognised analytical grade and only distilled water or water of equivalent purity. 4.1 Sulphuric acid, H2SO4( = 1,84 g/ml) 4.2 Nitric acid, HNO3( = 1,40 g/ml) 4.3 Sulphuric acid-nitric acid mixture While stirring, slowly add 300 ml of sulphuric acid (4.1) to 750 ml of water. Cool to ambient tempe

30、rature. While stirring, cautiously add 210 ml of nitric acid (4.2). 4.4 Sulphamic acid, H(NH2)SO34.5 Sulphamic acid solution, 100 g/l H(NH2)SO3Dissolve 10 g of sulphamic acid (4.4) in water and dilute to 100 ml. Prepare freshly before using. 4.6 Alcohol Ethanol: 95 % 0,2 %, methanol: min. 99,9 %, ot

31、her alcohols: higher than 99,9 %. DIN EN 16117-2:2013-02 EN 16117-2:2012 (E) 5 5 Apparatus 5.1 Current source Preferably use a 6 V accumulator. If a rectifier is to be used, an additional buffer battery is recommended. 5.2 Electrolysis equipment 5.2.1 Platinum cathode, Winkler type1), made preferabl

32、y from gauze containing approximately 400 meshes per square centimetre, woven from wire of diameter approximately 0,2 mm. The cathode shall be stiffened by doubling the gauze for about 3 mm at the top and the bottom of the cylinder or by reinforcing the gauze at the top and bottom with a platinum ba

33、nd or ring. The diameter of the cylinder shall be 30 mm to 50 mm and the height 40 mm to 60 mm. The stem shall be made from a platinum alloy wire such as platinum-iridium, platinum-rhodium or platinum-ruthenium, having a diameter of approximately 1,3 mm, flattened and welded the entire length of the

34、 gauze. The overall height of the cathode shall be approximately 130 mm. The cathode shall be sandblasted. 5.2.2 Spiral anode, made of platinum alloy wire of minimum diameter 1 mm, formed into a spiral of seven turns, having a height of approximately 50 mm and a diameter of 12 mm, the overall height

35、 being approximately 130 mm. The spiral section shall be sandblasted. 6 Sampling Sampling shall be carried out in accordance with ISO 1811-1 or ISO 1811-2, as appropriate. Test samples shall be in the form of fine drillings, chips or millings with a maximum thickness of 0,5 mm. 7 Procedure 7.1 Test

36、portion Weigh (5,0 0,001) g of the test sample. 7.2 Determination 7.2.1 Transfer the test portion (7.1) to a 400 ml tall-form beaker. Add 45 ml of the sulphuric acid-nitric acid mixture (4.3) by small portions and then cover with a watch glass. Cool if required to prevent the reaction from becoming

37、violent. When the reaction has subsided, heat moderately (80 C to 90 C) until dissolution is complete. Continue heating at approximately 90 C, without boiling, to completely expel the oxides of nitrogen (more than 1 h may be necessary). Cool slightly and carefully wash down the watch glass and the s

38、ides of the beaker with water. Add 10 ml of the sulphamic acid solution (4.5), stir and dilute to 175 ml to 200 ml. 7.2.2 Weigh the cathode (5.2.1) to the nearest 0,1 mg. 7.2.3 Position the electrodes (5.2.1 and 5.2.2) in the solution and add water so that the gauze is completely immersed. Cover the

39、 beaker with two halves of a watch glass, one of which has two indentations through which the electrode stems may pass. Electrolyze at a current of about 1 A to 3 A, slowly stirring the electrolyte by a magnetic stirrer, avoiding turbulence (see Note). When the solution becomes colourless, wash the

40、cover, the electrode stem and the sides of the beaker. Add 10 ml of sulphamic acid solution (4.5) and continue the electrolysis until deposition is essentially complete, as indicated by failure to plate on a new surface of the cathode stem, when the level of the solution is raised. NOTE When a curre

41、nt of 1 A to 3 A is used, the electrolysis requires less than 10 h. Avoid extended electrolysis times. 1)Platinum cathodes formed from plain or perforated sheets may also be used.DIN EN 16117-2:2013-02 EN 16117-2:2012 (E) 6 7.2.4 Without switching off the current, wash the cathode with a stream of w

42、ater as it is being removed from the spent solution. Immediately wash successively in two baths of water and two baths of ethanol, methanol or other alcohols (4.6). Dry at 110 C for 3 min to 5 min and cool to ambient temperature in a desiccator. Determine the mass of the metallic copper deposited. R

43、eserve the spent electrolyte. 7.2.5 Determine the residual copper in the spent electrolyte by a convenient spectrometric technique such as atomic absorption spectrometry or inductively coupled plasma optical emission spectrometry. The flame atomic absorption spectrometry method is described in the A

44、nnex A. 8 Expression of results Calculate the copper mass fraction, in percent (%), using Formula (1): wCu= 100)(0321+mmmm(1) where: wCuis the copper mass fraction in per cent (%); m0is the mass of the test portion (7.1), in grams (g); m1is the mass of the cathode plus the electrodeposited copper, i

45、n grams (g); m2is the mass of the cathode (5.2.1), in grams (g); m3is the mass of residual copper found in the spent electrolyte (Annex A), in grams (g). 9 Precision Twelve laboratories co-operated in testing this method and obtained the results summarised in Table 1. Table 1 Statistical information

46、 Level Reference value % Found % Repeatability r Reproducibility R 1 99,89 99,837 0,074 0,106 2 99,99 99,988 0,013 0,032 NOTE Taking into account the narrowness of the scope (99,80 % to 100 %) and the discrepancy in the relation between the level of content and the r and R levels (r and R for the lo

47、west level of content are higher than those for the highest level), the lg relationship between copper mass fraction (wCu) and r and R is irrelevant. Therefore, it is suitable to take 0,074 % and 0,106 % as the representative values for r and R respectively, for the whole scope of the method. DIN EN

48、 16117-2:2013-02 EN 16117-2:2012 (E) 7 10 Test report The test report shall contain the following information: a) identification of the test sample; b) reference to this European Standard (EN 16117-2); c) method used; d) results; e) any unusual characteristics noted during the determination; f) any

49、operation not included in this European Standard or in the document to which reference is made or regarded as optional; g) date of the test and/or date of preparation or signature of the test report; h) signature of the responsible person. DIN EN 16117-2:2013-02 EN 16117-2:2012 (E) 8 Annex A (normative) Spent electrolyte Determination of residual copper Flame atomic absorption spectrometric method (FAAS) A.1 General This Annex specifies a flame atomic absorp