DIN EN 15616-2013 Copper and copper alloys Determination of cadmium content Flame atomic absorption spectrometric method (FAAS) German version EN 15616 2012《铜和铜合金 镉含量的测定 火焰原子吸收光谱测定.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!$Fw“1943584www.din.deDDIN EN 15616Copper and copper alloys Determination of cadmium content Flame atomic absorption spectrometric method (FAAS);English version EN 15616:2012,English translation of DIN EN 15616:2013-02Kupfer und Kupferlegierungen Bestimmung des Cadmiumgehaltes Flammenatom

3、absorptionsspektrometrisches Verfahren (FAAS);Englische Fassung EN 15616:2012,Englische bersetzung von DIN EN 15616:2013-02Cuivre et alliages de cuivre Dtermination du cadmium Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF);Version anglaise EN 15616:2012,Traduction anglaise de DIN

4、 EN 15616:2013-02SupersedesDIN CEN/TS 15616:2009-07www.beuth.deDocument comprises 14 pagesIn case of doubt, the German-language original shall be considered authoritative.01.13DIN EN 15616:2013-02 2 A comma is used as the decimal marker. National foreword This document (EN 15616:2012) has been prepa

5、red by Technical Committee CEN/TC 133 “Copper and copper alloys” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Nichteisenmetalle (Nonferrous Metals Standards Committee), Working Committee NA 066-02-06 AA Analysenverfahren fr NE-Metalle.

6、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 ISO 5725-3 DIN ISO 5725-3 Amendments This standard differs from DIN CEN/TS 15616:2009-07 as follows: a) the standard has been converted into

7、 a European Standard; b) Clause 1 “Scope” has been updated; c) Clause 3 “Principle” has been completely revised and the dissolution process has been changed; d) Clause 9 “Precision” has been completely revised and the results of the precision test have been included. Previous editions DIN CEN/TS 156

8、16: 2009-07 National Annex 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 d

9、etermination of repeatability 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 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN

10、 15616 November 2012 ICS 77.120.30 Supersedes CEN/TS 15616:2009English Version Copper and copper alloys - Determination of cadmium content -Flame atomic absorption spectrometric method (FAAS) Cuivre et alliages de cuivre - Dtermination du cadmium - Mthode par spectromtrie dabsorption atomique dans l

11、a flamme (SAAF) Kupfer und Kupferlegierungen - Bestimmung des Cadmiumgehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) 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 condit

12、ions 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

13、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 standa

14、rds 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, Slov

15、enia, Spain, Sweden, Switzerland, Turkey and United 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 f

16、or CEN national Members. Ref. No. EN 15616:2012: EEN 15616:2012 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Sampling .57 Procedure .58 Expression of results 89 Precision 1010 Test report . 11Bibliography . 12DIN EN 15616:2013-02 EN 15616:2

17、012 (E) 3 Foreword This document (EN 15616:2012) 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 status of a national standard, either by publication of an identical text or by endorsem

18、ent, 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 patent rights. CEN and/or CENELEC shall not be held responsible for identifying any

19、or all such patent rights. This document supersedes CEN/TS 15616:2009. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to revise the following document: CEN/TS 15616:2009, Copper and copper alloys Determination of cadmium content Flame at

20、omic absorption spectrometric method (FAAS) In comparison with CEN/TS 15616:2009, the following significant technical changes were made: a) Conversion into a European Standard; b) Scope (Clause 1) revised; c) Principle (Clause 3) completely revised, dissolution process changed; d) Precision (Clause

21、9) completely revised and the results of the precision test included. 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

22、, 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 EN 15616:2013

23、-02 EN 15616:2012 (E) 4 1 Scope This European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the cadmium content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having cadmium mas

24、s fractions between 0,000 5 % and 0,1 %. 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

25、 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:

26、 Sampling of wrought products and castings 3 Principle Dissolution of a test portion in hydrochloric acid and nitric acid solution followed, after suitable dilution, by aspiration of the test solution into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of

27、the 228,8 nm line emitted by a cadmium hollow-cathode lamp. 4 Reagents During the analysis use only reagents of recognised analytical grade and only distilled water or water of equivalent purity. 4.1 Hydrochloric acid, HCl ( = 1,19 g/ml) 4.2 Nitric acid, HNO3( = 1,40 g/ml) 4.3 Nitric acid solution,

28、1 + 1 Add 500 ml of nitric acid (4.2) to 500 ml of water. 4.4 Cadmium stock solution, 1,0 g/l Cd Weigh (1 0,001) g of cadmium (Cd 99,8 %) and transfer it into a 250 ml beaker. Add 10 ml of nitric acid (4.2). Cover with a watch glass and, if necessary, heat gently to assist dissolution. When dissolut

29、ion is complete, allow to cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix. 1 ml of this solution contains 1,0 mg of Cd. 4.5 Cadmium standard solution, 0,005 g/l Cd Transfer 2,5 ml of cadmium stock solution (4.4) into a 50

30、0 ml one-mark volumetric flask. Dilute to the mark with water and mix. Prepare this solution immediately prior to use. 1 ml of this solution contains 0,005 mg of Cd. DIN EN 15616:2013-02 EN 15616:2012 (E) 5 4.6 Copper base solution, 50 g/l Cu Transfer 25,0 g of cadmium-free copper (Cu 99,95 %) into

31、a 1 000 ml beaker. Add 250 ml of hydrochloric acid (4.1) and, cautiously, 125 ml of nitric acid (4.2). Cover with a watch glass and heat gently until the copper has been completely dissolved, then heat up to the boiling point until the nitrous fumes have been expelled. Allow to cool and transfer the

32、 solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix. 4.7 Copper base solution, 5 g/l Cu Transfer 50,0 ml of copper base solution (4.6) into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix. 5 Apparatus 5.1 Atomic absorption

33、 spectrometer, fitted with an air/acetylene burner 5.2 Cadmium hollow-cathode lamp 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 Proce

34、dure 7.1 Preparation of the test portion solution 7.1.1 General Prepare test portion solutions in accordance with 7.1.2 or 7.1.3 depending on the expected cadmium content of the test sample. 7.1.2 Cadmium mass fractions between 0,000 5 % and 0,010 % Weigh (1 0,001) g of the test sample. Transfer the

35、 test portion into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of the nitric acid solution (4.3). Cover with a watch glass and heat gently until the test portion is completely dissolved and then bring to boiling point until the nitrous fumes have been expelled. Cool to room tempe

36、rature, and wash the beaker cover and the sides of the beaker with water. Transfer the dissolved test portion quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix. NOTE The validation test of this method showed that for cadmium mass fractions until and includ

37、ing 0,01 %, the results are better when the determination is carried out following 7.1.2. 7.1.3 Cadmium mass fractions between 0,01 % and 0,10 % Weigh (1 0,001) g of the test sample. Transfer the test portion into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of the nitric acid sol

38、ution (4.3). Cover with a watch glass and heat gently until the test portion is completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, and wash the beaker cover and the sides of the beaker with water. DIN EN 15616:2013-02 EN 156

39、16:2012 (E) 6 Transfer the dissolved test portion quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix. Transfer 5,0 ml of this solution into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix. 7.2 Blank test Carry out a blank test simu

40、ltaneously with the determination, following the same procedure and using the same quantities of all reagents as used for the determination, but substituting pure copper for the test portion. 7.3 Check test Make a preliminary check of the apparatus by preparing a solution of a reference material or

41、a synthetic sample containing a known amount of cadmium and of a composition similar to the material to be analysed. Carry out the procedure specified in 7.5. 7.4 Establishment of the calibration curve 7.4.1 Preparation of the calibration solutions 7.4.1.1 General In all cases, copper, chloride and

42、nitrate concentrations, and acidity in the calibration solutions shall be similar to those of the test portion solutions. The presence of copper in the calibration solutions compensates for chemical interaction effects of copper in the test portion solution. Normally no similar additions are require

43、d to compensate for the effect of alloying elements. If an alloying element is present in the material to be analysed in mass fraction 10 %, an appropriate mass of this element shall be added to the calibration solutions. The volumes of copper base solution added (4.6 or 4.7) have been calculated to

44、 compensate for chemical interaction effects of copper in test solutions of copper or high-copper alloys. Over-compensation may occur if the same volumes are added when the test samples are copper-based alloys where the percentage of copper is lower. In these cases, the volumes of copper base soluti

45、on shall be decreased to match the copper content of the test sample in solution. The cadmium concentration of the calibration solutions shall be adjusted to suit the sensitivity of the spectrometer used, so that the curve of absorbance as a function of concentration is a straight line. 7.4.1.2 Cadm

46、ium mass fractions between 0,000 5 % and 0,010 % Into each of a series of five 100 ml one-mark volumetric flasks, introduce the volumes of cadmium standard solution (4.5) and copper base solution (4.6) shown in Table 1. Dilute to the mark with water and mix. DIN EN 15616:2013-02 EN 15616:2012 (E) 7

47、Table 1 Calibration for cadmium mass fractions between 0,000 5 % and 0,010 % Cadmium Corresponding Corresponding Copper Corresponding Correspondingstandard cadmium cadmium base copper cadmiumsolution volume mass concentration solution volume mass mass fraction(4.5) after final dilution (4.6) of samp

48、leml mg g/ml ml g % 0a0 0 20 1 0 1 0,005 0,05 20 1 0,000 5 4 0,020 0,20 20 1 0,002 010 0,050 0,50 20 1 0,005 0 20 0,100 1,00 20 1 0,010 0aBlank test on reagents for calibration curve. 7.4.1.3 Cadmium mass fractions between 0,01 % and 0,10 % Into each of a series of five 100 ml one-mark volumetric fl

49、asks, introduce the volumes of cadmium standard solution (4.5) and copper base solution (4.7) shown in Table 2. Dilute to the mark with water and mix. Table 2 Calibration for cadmium mass fractions between 0,01 % and 0,10 % Cadmium Corresponding Corresponding Copper Corresponding Correspondingstandard cadmium cadmium base copper cadmiumsolution volume mass concentration solution volume mass mass fraction(4.5) after final dilution (4.7) of sampleml mg g/ml ml g % 0a0 0 10 0,05 0 1 0,