EN 15616-2012 en Copper and copper alloys - Determination of cadmium content - Flame atomic absorption spectrometric method (FAAS)《铜和铜合金-镉含量的测定-火焰原子吸收光谱法(FAAS)》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15616:2012Copper and copper alloys Determination of cadmiumcontent Flame atomicabsorption spectrometricmethod (FAAS)BS EN 15616:2012 BRITISH STANDARDNational forewordThis B

2、ritish Standard is the UK implementation of EN 15616:2012. It supersedes DD CEN/TS 15616:2009 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee NFE/34, Copper and copper alloys.A list of organizations represented on this committee can be obtained on requ

3、est to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2013. Published by BSI Standards Limited 2013ISBN 978 0 580 75026 7 ICS 77.120.30 Compliance with a Briti

4、sh Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2013.Amendments issued since publicationDate T e x t a f f e c t e dBS EN 15616:2012EUROPEAN STANDARD NORME EUROPENNE EUROPI

5、SCHE NORM EN 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 ato

6、mique dans la 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 stipulat

7、e 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 Stan

8、dard 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 nat

9、ional 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, Sl

10、ovakia, Slovenia, 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

11、 worldwide for CEN national Members. Ref. No. EN 15616:2012: EBS EN 15616:2012EN 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 . 12BS

12、EN 15616:2012EN 15616:2012 (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 identi

13、cal 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 patent rights. CEN and/or CENELEC shall not be held responsib

14、le for identifying any 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 c

15、admium content Flame atomic 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

16、; d) Precision (Clause 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,

17、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 Kin

18、gdom. BS EN 15616:2012EN 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

19、having cadmium mass 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 lat

20、est 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 chemica

21、l analysis Part 2: 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

22、the absorption of 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 Nitr

23、ic acid solution, 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 dissolut

24、ion. When dissolution 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 soluti

25、on (4.4) into a 500 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. BS EN 15616:2012EN 15616:2012 (E) 5 4.6 Copper base solution, 50 g/l Cu Transfer 25,0 g of cadmium-free copper (Cu 9

26、9,95 %) into 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

27、 transfer the 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 Atom

28、ic absorption 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,

29、5 mm. 7 Procedure 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.

30、 Transfer the 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

31、to room temperature, 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 unt

32、il and including 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 ni

33、tric acid solution (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. BS EN 15616:20

34、12EN 15616:2012 (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 t

35、est simultaneously 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 mate

36、rial or 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, chlor

37、ide and 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

38、 required 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 calcu

39、lated to 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 bas

40、e solution 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.

41、1.2 Cadmium 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. BS EN 15616:2012EN 15616:2012 (E)

42、 7 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 s

43、ampleml 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

44、 flasks, 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 Correspondingsta

45、ndard 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 0,005 0,05 10 0,05 0,01 3 0,015 0,15 10 0,05 0,036 0,030 0,30 10 0,05 0,06 10 0,050 0,50 10 0,05 0,10aBlank test

46、 on reagents for calibration curve. 7.4.2 Adjustment of the atomic absorption spectrometer Fit the cadmium hollow-cathode lamp (5.2) to the atomic absorption spectrometer (5.1), switch on the current and allow it to stabilise. Adjust the wavelength in the region of 228,8 nm to minimum absorbance. Fo

47、llowing manufacturers instructions, fit the correct burner, light the flame and allow the burner temperature to stabilise. Taking careful note of the manufacturers instructions regarding the minimum flow rate of acetylene, aspirate the calibration solution of highest concentration of analyte and adj

48、ust the burner configuration and gas flows to obtain maximum absorbance. 7.4.3 Spectrometric measurement of the calibration solutions Aspirate the relevant series of calibration solutions (7.4.1.2 or 7.4.1.3 depending on the expected cadmium content) in succession, into the flame and measure the abs

49、orbance for each. Take care to keep the aspiration rate constant throughout the preparation of the calibration curve. Spray water through the burner after each measurement, see NOTE. NOTE For certain types of apparatus, instead of water it is preferable to use a solution containing the attack reagents, in the same concentrations as in the test portion solutions. BS EN 15616:2012EN 15616:2012 (E) 8 7.4.4 Calibration curve Establish the calibration curve using measured absorbances and corresponding ana